data_feynmanite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'feynmanite' _chemical_compound_source 'Markey mine, Utah' _chemical_formula_sum 'H8 Na0.97 O10.50 S U' _chemical_formula_weight 468.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_H-M_alt 'P 2/n' _space_group_name_Hall '-P 2yac' _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+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 6.927(3) _cell_length_b 8.355(4) _cell_length_c 16.210(7) _cell_angle_alpha 90 _cell_angle_beta 90.543(4) _cell_angle_gamma 90 _cell_volume 938.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _exptl_crystal_density_diffrn 3.316 _exptl_crystal_F_000 843 _exptl_crystal_size_max 0.068 _exptl_crystal_size_mid 0.061 _exptl_crystal_size_min 0.005 _exptl_absorpt_coefficient_mu 17.606 _shelx_estimated_absorpt_T_min 0.381 _shelx_estimated_absorpt_T_max 0.917 _exptl_absorpt_correction_type multi-scan _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'microfocus sealed tube' _diffrn_measurement_device_type 'Bruker Apex II Quazar' _diffrn_measurement_method 'Apex II CCD-based detector' _diffrn_reflns_number 10605 _diffrn_reflns_av_unetI/netI 0.0445 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.438 _diffrn_reflns_theta_max 29.029 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.941 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.941 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.941 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 2358 _reflns_number_gt 1879 _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_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _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^)+(0.0537P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2358 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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_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 U U 0.74439(4) 0.40606(4) 0.36948(2) 0.01707(11) Uani 1 1 d . . . . . S S 0.2468(3) 0.5059(3) 0.41111(11) 0.0210(4) Uani 1 1 d . . . . . Na1 Na 0.7160(12) -0.0931(9) 0.3631(5) 0.035(3) Uani 0.48(2) 1 d . . P . . Na2 Na 0.250000 0.8584(10) 0.250000 0.027(3) Uani 0.598(19) 2 d S T P . . Na3 Na 0.779(3) -0.109(2) 0.6233(11) 0.036(9) Uani 0.19(2) 1 d . . P . . O1 O 0.2378(9) 0.5987(8) 0.3348(4) 0.0324(15) Uani 1 1 d . . . . . O2 O 0.2596(8) 0.6163(7) 0.4820(3) 0.0270(14) Uani 1 1 d . . . . . O3 O 0.4148(8) 0.3956(7) 0.4119(4) 0.0266(13) Uani 1 1 d . . . . . O4 O 0.0725(8) 0.4033(7) 0.4196(3) 0.0269(13) Uani 1 1 d . . . . . O5 O 0.7405(7) 0.6170(7) 0.3759(3) 0.0224(13) Uani 1 1 d . . . . . O6 O 0.7480(7) 0.1942(7) 0.3653(3) 0.0239(13) Uani 1 1 d . . . . . OH O 0.5595(7) 0.4159(7) 0.2483(3) 0.0233(12) Uani 1 1 d . . . . . OW1 O 0.8389(18) -0.0953(10) 0.4966(7) 0.083(3) Uani 1 1 d . . . . . OW2 O 0.250000 1.1657(16) 0.250000 0.084(5) Uani 1 2 d S T P . . OW3 O 0.422(2) -0.0885(11) 0.3955(7) 0.096(4) Uani 1 1 d . . . . . OW4A O 0.921(6) -0.109(2) 0.2828(11) 0.050(9) Uani 0.52(7) 1 d . . P . . OW4B O 0.027(6) 0.888(3) 0.2917(18) 0.071(8) Uani 0.48(7) 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 U 0.01353(16) 0.02393(18) 0.01374(16) -0.00056(12) -0.00060(10) 0.00003(12) S 0.0131(9) 0.0384(13) 0.0115(8) -0.0005(8) 0.0001(7) 0.0003(8) Na1 0.036(5) 0.022(5) 0.047(6) 0.002(3) 0.001(4) 0.007(3) Na2 0.017(4) 0.031(5) 0.033(5) 0.000 0.005(3) 0.000 Na3 0.058(16) 0.023(12) 0.027(12) -0.002(8) 0.008(10) -0.009(9) O1 0.036(4) 0.045(4) 0.016(3) 0.006(3) 0.000(2) -0.002(3) O2 0.024(3) 0.042(4) 0.015(3) 0.000(2) 0.002(2) -0.007(3) O3 0.016(3) 0.035(4) 0.029(3) 0.004(3) 0.003(2) 0.002(2) O4 0.016(3) 0.042(4) 0.023(3) 0.000(3) -0.002(2) -0.001(2) O5 0.020(3) 0.023(3) 0.024(3) -0.001(2) 0.001(2) 0.000(2) O6 0.021(3) 0.030(4) 0.020(3) -0.002(2) -0.001(2) -0.001(3) OH 0.014(2) 0.041(4) 0.015(2) -0.002(2) 0.002(2) 0.003(2) OW1 0.123(10) 0.048(6) 0.076(7) -0.002(5) -0.019(7) -0.010(5) OW2 0.098(11) 0.050(8) 0.103(11) 0.000 -0.044(9) 0.000 OW3 0.142(11) 0.050(6) 0.096(8) -0.001(5) -0.022(8) -0.014(6) OW4A 0.04(2) 0.050(11) 0.059(11) 0.010(7) 0.013(9) -0.013(9) OW4B 0.017(16) 0.062(13) 0.14(2) 0.033(12) 0.013(12) 0.003(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O5 1.766(6) . ? U O6 1.771(6) . ? U OH 2.337(5) . ? U OH 2.355(5) 2_655 ? U O3 2.392(6) . ? U O4 2.406(5) 1_655 ? U O2 2.416(5) 3_666 ? U U 3.8752(17) 2_655 ? U Na3 4.13(2) 3_756 ? S O1 1.461(6) . ? S O2 1.475(6) . ? S O3 1.484(6) . ? S O4 1.488(6) . ? S Na3 3.370(19) 3_656 ? Na1 OW4A 1.94(3) . ? Na1 OW3 2.108(17) . ? Na1 OW1 2.319(13) . ? Na1 O6 2.411(9) . ? Na1 O5 2.437(9) 1_545 ? Na1 OW4B 2.46(4) 1_645 ? Na1 OW4A 2.54(3) 2_655 ? Na1 OW4B 3.01(4) 2_545 ? Na1 Na1 3.702(16) 2_655 ? Na1 Na2 3.719(9) 1_545 ? Na1 Na3 3.83(2) 3_656 ? Na1 Na3 3.89(2) 3_756 ? Na2 OW4B 1.71(3) . ? Na2 OW4B 1.71(3) 2 ? Na2 OW4A 2.36(4) 2_665 ? Na2 OW4A 2.36(4) 1_465 ? Na2 OW2 2.567(16) . ? Na2 O1 2.570(9) 2 ? Na2 O1 2.570(9) . ? Na2 OW3 2.670(12) 1_565 ? Na2 OW3 2.670(12) 2_565 ? Na2 Na3 2.94(2) 3_666 ? Na2 Na3 2.94(2) 4_565 ? Na3 OW1 2.10(2) . ? Na3 OW2 2.120(19) 3_666 ? Na3 OW3 2.18(2) 3_656 ? Na3 OW4B 2.66(4) 3_666 ? Na3 O4 2.76(2) 3_656 ? Na3 O3 2.804(19) 3_656 ? Na3 Na3 4.13(4) 2_656 ? OW4A OW4B 0.75(2) 1_645 ? 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 O5 U O6 178.8(2) . . ? O5 U OH 90.3(2) . . ? O6 U OH 90.6(2) . . ? O5 U OH 91.3(2) . 2_655 ? O6 U OH 89.7(2) . 2_655 ? OH U OH 68.5(2) . 2_655 ? O5 U O3 90.2(2) . . ? O6 U O3 89.3(2) . . ? OH U O3 74.09(19) . . ? OH U O3 142.54(19) 2_655 . ? O5 U O4 90.3(2) . 1_655 ? O6 U O4 89.4(2) . 1_655 ? OH U O4 142.41(19) . 1_655 ? OH U O4 73.94(18) 2_655 1_655 ? O3 U O4 143.49(19) . 1_655 ? O5 U O2 91.1(2) . 3_666 ? O6 U O2 87.8(2) . 3_666 ? OH U O2 146.05(19) . 3_666 ? OH U O2 145.37(19) 2_655 3_666 ? O3 U O2 71.99(19) . 3_666 ? O4 U O2 71.50(19) 1_655 3_666 ? O5 U U 93.38(16) . 2_655 ? O6 U U 87.77(15) . 2_655 ? OH U U 34.46(13) . 2_655 ? OH U U 34.16(13) 2_655 2_655 ? O3 U U 108.39(14) . 2_655 ? O4 U U 108.02(14) 1_655 2_655 ? O2 U U 175.53(15) 3_666 2_655 ? O5 U Na3 127.7(3) . 3_756 ? O6 U Na3 52.3(3) . 3_756 ? OH U Na3 118.4(3) . 3_756 ? OH U Na3 65.0(3) 2_655 3_756 ? O3 U Na3 137.2(3) . 3_756 ? O4 U Na3 39.9(3) 1_655 3_756 ? O2 U Na3 86.7(3) 3_666 3_756 ? U U Na3 90.3(3) 2_655 3_756 ? O1 S O2 109.2(4) . . ? O1 S O3 111.3(4) . . ? O2 S O3 109.9(3) . . ? O1 S O4 110.8(4) . . ? O2 S O4 109.3(3) . . ? O3 S O4 106.2(3) . . ? O1 S Na3 112.4(4) . 3_656 ? O2 S Na3 138.4(4) . 3_656 ? O3 S Na3 55.3(5) . 3_656 ? O4 S Na3 53.5(4) . 3_656 ? OW4A Na1 OW3 152.0(12) . . ? OW4A Na1 OW1 111.2(12) . . ? OW3 Na1 OW1 96.6(5) . . ? OW4A Na1 O6 90.7(6) . . ? OW3 Na1 O6 93.8(4) . . ? OW1 Na1 O6 87.8(3) . . ? OW4A Na1 O5 86.4(6) . 1_545 ? OW3 Na1 O5 93.6(4) . 1_545 ? OW1 Na1 O5 83.6(3) . 1_545 ? O6 Na1 O5 169.2(4) . 1_545 ? OW4A Na1 OW4B 14.2(9) . 1_645 ? OW3 Na1 OW4B 166.1(11) . 1_645 ? OW1 Na1 OW4B 97.1(10) . 1_645 ? O6 Na1 OW4B 89.4(6) . 1_645 ? O5 Na1 OW4B 85.2(6) 1_545 1_645 ? OW4A Na1 OW4A 68.9(19) . 2_655 ? OW3 Na1 OW4A 83.2(10) . 2_655 ? OW1 Na1 OW4A 176.5(6) . 2_655 ? O6 Na1 OW4A 95.7(5) . 2_655 ? O5 Na1 OW4A 92.9(5) 1_545 2_655 ? OW4B Na1 OW4A 83.0(17) 1_645 2_655 ? OW4A Na1 OW4B 81.0(16) . 2_545 ? OW3 Na1 OW4B 71.0(8) . 2_545 ? OW1 Na1 OW4B 167.0(8) . 2_545 ? O6 Na1 OW4B 96.6(5) . 2_545 ? O5 Na1 OW4B 93.2(5) 1_545 2_545 ? OW4B Na1 OW4B 95.2(13) 1_645 2_545 ? OW4A Na1 OW4B 12.2(6) 2_655 2_545 ? OW4A Na1 Na1 40.0(11) . 2_655 ? OW3 Na1 Na1 112.3(5) . 2_655 ? OW1 Na1 Na1 151.1(6) . 2_655 ? O6 Na1 Na1 90.1(2) . 2_655 ? O5 Na1 Na1 94.3(2) 1_545 2_655 ? OW4B Na1 Na1 54.1(9) 1_645 2_655 ? OW4A Na1 Na1 29.3(9) 2_655 2_655 ? OW4B Na1 Na1 41.5(6) 2_545 2_655 ? OW4A Na1 Na2 107.4(11) . 1_545 ? OW3 Na1 Na2 44.7(4) . 1_545 ? OW1 Na1 Na2 140.2(4) . 1_545 ? O6 Na1 Na2 101.2(3) . 1_545 ? O5 Na1 Na2 89.6(3) 1_545 1_545 ? OW4B Na1 Na2 121.4(10) 1_645 1_545 ? OW4A Na1 Na2 38.9(9) 2_655 1_545 ? OW4B Na1 Na2 26.9(6) 2_545 1_545 ? Na1 Na1 Na2 68.3(2) 2_655 1_545 ? OW4A Na1 Na3 136.9(11) . 3_656 ? OW3 Na1 Na3 27.1(4) . 3_656 ? OW1 Na1 Na3 105.7(5) . 3_656 ? O6 Na1 Na3 69.1(3) . 3_656 ? O5 Na1 Na3 119.6(4) 1_545 3_656 ? OW4B Na1 Na3 147.6(7) 1_645 3_656 ? OW4A Na1 Na3 75.6(8) 2_655 3_656 ? OW4B Na1 Na3 65.0(7) 2_545 3_656 ? Na1 Na1 Na3 100.3(4) 2_655 3_656 ? Na2 Na1 Na3 45.8(3) 1_545 3_656 ? OW4A Na1 Na3 53.5(9) . 3_756 ? OW3 Na1 Na3 148.0(5) . 3_756 ? OW1 Na1 Na3 68.2(4) . 3_756 ? O6 Na1 Na3 59.0(4) . 3_756 ? O5 Na1 Na3 111.4(4) 1_545 3_756 ? OW4B Na1 Na3 42.5(9) 1_645 3_756 ? OW4A Na1 Na3 113.7(10) 2_655 3_756 ? OW4B Na1 Na3 124.4(6) 2_545 3_756 ? Na1 Na1 Na3 86.2(4) 2_655 3_756 ? Na2 Na1 Na3 148.4(4) 1_545 3_756 ? Na3 Na1 Na3 127.7(6) 3_656 3_756 ? OW4B Na2 OW4B 163.4(17) . 2 ? OW4B Na2 OW4A 161.8(11) . 2_665 ? OW4B Na2 OW4A 10.5(12) 2 2_665 ? OW4B Na2 OW4A 10.5(12) . 1_465 ? OW4B Na2 OW4A 161.8(11) 2 1_465 ? OW4A Na2 OW4A 166.9(9) 2_665 1_465 ? OW4B Na2 OW2 81.7(9) . . ? OW4B Na2 OW2 81.7(9) 2 . ? OW4A Na2 OW2 83.5(5) 2_665 . ? OW4A Na2 OW2 83.5(5) 1_465 . ? OW4B Na2 O1 111.6(12) . 2 ? OW4B Na2 O1 82.9(7) 2 2 ? OW4A Na2 O1 86.5(5) 2_665 2 ? OW4A Na2 O1 104.7(5) 1_465 2 ? OW2 Na2 O1 147.60(17) . 2 ? OW4B Na2 O1 82.9(7) . . ? OW4B Na2 O1 111.6(12) 2 . ? OW4A Na2 O1 104.7(5) 2_665 . ? OW4A Na2 O1 86.5(5) 1_465 . ? OW2 Na2 O1 147.60(17) . . ? O1 Na2 O1 64.8(3) 2 . ? OW4B Na2 OW3 91.4(13) . 1_565 ? OW4B Na2 OW3 85.9(12) 2 1_565 ? OW4A Na2 OW3 75.9(6) 2_665 1_565 ? OW4A Na2 OW3 101.9(6) 1_465 1_565 ? OW2 Na2 OW3 80.4(3) . 1_565 ? O1 Na2 OW3 126.6(4) 2 1_565 ? O1 Na2 OW3 71.6(3) . 1_565 ? OW4B Na2 OW3 85.9(12) . 2_565 ? OW4B Na2 OW3 91.4(13) 2 2_565 ? OW4A Na2 OW3 101.9(6) 2_665 2_565 ? OW4A Na2 OW3 75.9(6) 1_465 2_565 ? OW2 Na2 OW3 80.4(3) . 2_565 ? O1 Na2 OW3 71.6(3) 2 2_565 ? O1 Na2 OW3 126.6(4) . 2_565 ? OW3 Na2 OW3 160.9(5) 1_565 2_565 ? OW4B Na2 Na3 63.4(13) . 3_666 ? OW4B Na2 Na3 104.0(9) 2 3_666 ? OW4A Na2 Na3 98.6(7) 2_665 3_666 ? OW4A Na2 Na3 71.8(6) 1_465 3_666 ? OW2 Na2 Na3 44.7(4) . 3_666 ? O1 Na2 Na3 167.7(4) 2 3_666 ? O1 Na2 Na3 103.0(4) . 3_666 ? OW3 Na2 Na3 45.4(5) 1_565 3_666 ? OW3 Na2 Na3 117.8(5) 2_565 3_666 ? OW4B Na2 Na3 104.0(9) . 4_565 ? OW4B Na2 Na3 63.4(13) 2 4_565 ? OW4A Na2 Na3 71.8(6) 2_665 4_565 ? OW4A Na2 Na3 98.6(7) 1_465 4_565 ? OW2 Na2 Na3 44.7(4) . 4_565 ? O1 Na2 Na3 103.0(4) 2 4_565 ? O1 Na2 Na3 167.7(4) . 4_565 ? OW3 Na2 Na3 117.8(5) 1_565 4_565 ? OW3 Na2 Na3 45.4(5) 2_565 4_565 ? Na3 Na2 Na3 89.3(8) 3_666 4_565 ? OW4B Na2 Na1 124.9(13) . 1_565 ? OW4B Na2 Na1 52.9(13) 2 1_565 ? OW4A Na2 Na1 42.6(6) 2_665 1_565 ? OW4A Na2 Na1 135.4(6) 1_465 1_565 ? OW2 Na2 Na1 83.75(17) . 1_565 ? O1 Na2 Na1 108.8(2) 2 1_565 ? O1 Na2 Na1 82.0(2) . 1_565 ? OW3 Na2 Na1 33.7(3) 1_565 1_565 ? OW3 Na2 Na1 142.7(4) 2_565 1_565 ? Na3 Na2 Na1 69.1(5) 3_666 1_565 ? Na3 Na2 Na1 101.6(5) 4_565 1_565 ? OW1 Na3 OW2 168.6(12) . 3_666 ? OW1 Na3 OW3 87.4(8) . 3_656 ? OW2 Na3 OW3 103.8(10) 3_666 3_656 ? OW1 Na3 OW4B 111.5(10) . 3_666 ? OW2 Na3 OW4B 72.9(8) 3_666 3_666 ? OW3 Na3 OW4B 82.4(9) 3_656 3_666 ? OW1 Na3 O4 74.0(6) . 3_656 ? OW2 Na3 O4 94.7(8) 3_666 3_656 ? OW3 Na3 O4 151.5(9) 3_656 3_656 ? OW4B Na3 O4 124.2(11) 3_666 3_656 ? OW1 Na3 O3 86.9(7) . 3_656 ? OW2 Na3 O3 87.4(7) 3_666 3_656 ? OW3 Na3 O3 108.2(9) 3_656 3_656 ? OW4B Na3 O3 159.6(9) 3_666 3_656 ? O4 Na3 O3 50.6(4) 3_656 3_656 ? OW1 Na3 Na2 131.3(8) . 3_666 ? OW2 Na3 Na2 58.3(6) 3_666 3_666 ? OW3 Na3 Na2 60.8(6) 3_656 3_666 ? OW4B Na3 Na2 35.1(7) 3_666 3_666 ? O4 Na3 Na2 147.0(8) 3_656 3_666 ? O3 Na3 Na2 135.6(8) 3_656 3_666 ? OW1 Na3 S 84.4(6) . 3_656 ? OW2 Na3 S 86.2(7) 3_666 3_656 ? OW3 Na3 S 133.5(9) 3_656 3_656 ? OW4B Na3 S 142.7(10) 3_666 3_656 ? O4 Na3 S 25.7(2) 3_656 3_656 ? O3 Na3 S 25.8(2) 3_656 3_656 ? Na2 Na3 S 144.3(6) 3_666 3_656 ? OW1 Na3 Na1 102.5(8) . 3_656 ? OW2 Na3 Na1 87.1(7) 3_666 3_656 ? OW3 Na3 Na1 26.2(5) 3_656 3_656 ? OW4B Na3 Na1 96.4(9) 3_666 3_656 ? O4 Na3 Na1 138.0(7) 3_656 3_656 ? O3 Na3 Na1 87.7(6) 3_656 3_656 ? Na2 Na3 Na1 65.1(5) 3_666 3_656 ? S Na3 Na1 113.3(6) 3_656 3_656 ? OW1 Na3 Na1 81.2(7) . 3_756 ? OW2 Na3 Na1 97.9(7) 3_666 3_756 ? OW3 Na3 Na1 104.7(7) 3_656 3_756 ? OW4B Na3 Na1 38.8(7) 3_666 3_756 ? O4 Na3 Na1 93.7(6) 3_656 3_756 ? O3 Na3 Na1 144.3(8) 3_656 3_756 ? Na2 Na3 Na1 73.7(4) 3_666 3_756 ? S Na3 Na1 118.9(6) 3_656 3_756 ? Na1 Na3 Na1 127.7(6) 3_656 3_756 ? OW1 Na3 U 84.0(7) . 3_756 ? OW2 Na3 U 85.5(7) 3_666 3_756 ? OW3 Na3 U 165.7(8) 3_656 3_756 ? OW4B Na3 U 90.2(9) 3_666 3_756 ? O4 Na3 U 34.1(3) 3_656 3_756 ? O3 Na3 U 82.7(5) 3_656 3_756 ? Na2 Na3 U 117.9(6) 3_666 3_756 ? S Na3 U 56.9(3) 3_656 3_756 ? Na1 Na3 U 168.1(6) 3_656 3_756 ? Na1 Na3 U 62.7(4) 3_756 3_756 ? OW1 Na3 Na3 173.5(11) . 2_656 ? OW2 Na3 Na3 13.0(6) 3_666 2_656 ? OW3 Na3 Na3 94.0(7) 3_656 2_656 ? OW4B Na3 Na3 62.5(7) 3_666 2_656 ? O4 Na3 Na3 106.9(5) 3_656 2_656 ? O3 Na3 Na3 98.7(5) 3_656 2_656 ? Na2 Na3 Na3 45.3(4) 3_666 2_656 ? S Na3 Na3 99.1(3) 3_656 2_656 ? Na1 Na3 Na3 81.2(6) 3_656 2_656 ? Na1 Na3 Na3 92.3(6) 3_756 2_656 ? U Na3 Na3 93.3(6) 3_756 2_656 ? S O1 Na2 154.1(4) . . ? S O2 U 136.6(4) . 3_666 ? S O3 U 136.5(3) . . ? S O3 Na3 98.9(6) . 3_656 ? U O3 Na3 115.5(5) . 3_656 ? S O4 U 136.7(3) . 1_455 ? S O4 Na3 100.8(5) . 3_656 ? U O4 Na3 106.0(5) 1_455 3_656 ? U O5 Na1 171.2(3) . 1_565 ? U O6 Na1 173.8(3) . . ? U OH U 111.4(2) . 2_655 ? Na3 OW1 Na1 147.0(9) . . ? Na3 OW2 Na3 154.0(12) 4_565 3_666 ? Na3 OW2 Na2 77.0(6) 4_565 . ? Na3 OW2 Na2 77.0(6) 3_666 . ? Na1 OW3 Na3 126.7(7) . 3_656 ? Na1 OW3 Na2 101.6(5) . 1_545 ? Na3 OW3 Na2 73.8(6) 3_656 1_545 ? OW4B OW4A Na1 127(3) 1_645 . ? OW4B OW4A Na2 25(3) 1_645 1_645 ? Na1 OW4A Na2 150.8(16) . 1_645 ? OW4B OW4A Na1 122(3) 1_645 2_655 ? Na1 OW4A Na1 110.7(19) . 2_655 ? Na2 OW4A Na1 98.5(8) 1_645 2_655 ? OW4A OW4B Na2 145(4) 1_465 . ? OW4A OW4B Na1 39(2) 1_465 1_465 ? Na2 OW4B Na1 173.5(14) . 1_465 ? OW4A OW4B Na3 125(3) 1_465 3_666 ? Na2 OW4B Na3 81.5(17) . 3_666 ? Na1 OW4B Na3 98.7(10) 1_465 3_666 ? OW4A OW4B Na1 45(3) 1_465 2_565 ? Na2 OW4B Na1 100.3(12) . 2_565 ? Na1 OW4B Na1 84.4(13) 1_465 2_565 ? Na3 OW4B Na1 132.2(9) 3_666 2_565 ? _refine_diff_density_max 3.761 _refine_diff_density_min -2.502 _refine_diff_density_rms 0.341 _shelx_res_file ; TITL JM21870_a.res in P2/n feyn.res created by SHELXL-2016/6 at 20:29:20 on 23-Mar-2017 REM Old TITL JM21870 in P2/n REM SHELXT solution in P2/n REM R1 0.084, Rweak 0.002, Alpha 0.027, Orientation as input REM Formula found by SHELXT: O10 S U CELL 0.71073 6.9270 8.3548 16.2100 90.000 90.543 90.000 ZERR 4.000 0.0029 0.0035 0.0067 0.000 0.004 0.000 LATT 1 SYMM 1/2-X, Y, 1/2-Z SFAC O NA S U H UNIT 42 3.87 4 4 32 TEMP 25.000 L.S. 10 FMAP 2 PLAN 10 ACTA SIZE 0.068 0.061 0.005 WGHT 0.053700 FVAR 0.22000 0.48175 0.59798 0.37233 0.52090 U 4 0.744388 0.406060 0.369485 11.00000 0.01353 0.02393 = 0.01374 -0.00056 -0.00060 0.00003 S 3 0.246796 0.505918 0.411106 11.00000 0.01310 0.03844 = 0.01149 -0.00054 0.00007 0.00025 NA1 2 0.715978 -0.093110 0.363117 21.00000 0.03614 0.02207 = 0.04679 0.00211 0.00054 0.00683 NA2 2 0.250000 0.858442 0.250000 30.50000 0.01652 0.03054 = 0.03332 0.00000 0.00488 0.00000 NA3 2 0.779310 -0.108697 0.623273 40.50000 0.05828 0.02260 = 0.02727 -0.00243 0.00794 -0.00900 O1 1 0.237752 0.598676 0.334763 11.00000 0.03568 0.04523 = 0.01643 0.00587 -0.00002 -0.00231 O2 1 0.259599 0.616322 0.481961 11.00000 0.02432 0.04160 = 0.01508 0.00014 0.00171 -0.00686 O3 1 0.414759 0.395613 0.411894 11.00000 0.01598 0.03491 = 0.02902 0.00415 0.00260 0.00176 O4 1 0.072526 0.403345 0.419560 11.00000 0.01581 0.04211 = 0.02267 0.00042 -0.00219 -0.00125 O5 1 0.740455 0.616998 0.375863 11.00000 0.01994 0.02301 = 0.02422 -0.00056 0.00078 -0.00043 O6 1 0.747966 0.194212 0.365282 11.00000 0.02096 0.03037 = 0.02023 -0.00227 -0.00099 -0.00103 OH 1 0.559479 0.415888 0.248273 11.00000 0.01383 0.04098 = 0.01519 -0.00237 0.00179 0.00277 OW1 1 0.838906 -0.095263 0.496647 11.00000 0.12344 0.04802 = 0.07638 -0.00242 -0.01944 -0.01010 OW2 1 0.250000 1.165686 0.250000 10.50000 0.09766 0.05016 = 0.10287 0.00000 -0.04366 0.00000 OW3 1 0.422111 -0.088491 0.395546 11.00000 0.14183 0.04975 = 0.09630 -0.00110 -0.02244 -0.01413 OW4A 1 0.920662 -0.109333 0.282825 51.00000 0.04201 0.05005 = 0.05940 0.01026 0.01301 -0.01261 OW4B 1 0.027252 0.888042 0.291662 -51.00000 0.01680 0.06195 = 0.13548 0.03272 0.01316 0.00344 HKLF 4 REM JM21870_a.res in P2/n REM R1 = 0.0371 for 1879 Fo > 4sig(Fo) and 0.0537 for all 2358 data REM 150 parameters refined using 0 restraints END WGHT 0.0537 0.0000 REM Highest difference peak 3.761, deepest hole -2.502, 1-sigma level 0.341 Q1 1 0.7408 0.3016 0.3664 11.00000 0.05 3.76 Q2 1 0.7426 0.5129 0.3679 11.00000 0.05 3.67 Q3 1 0.7437 -0.2211 0.3671 11.00000 0.05 2.67 Q4 1 0.2610 0.5992 0.3928 11.00000 0.05 2.01 Q5 1 0.2509 0.3301 0.4149 11.00000 0.05 1.48 Q6 1 0.8108 0.4064 0.3363 11.00000 0.05 1.48 Q7 1 0.7805 0.4032 0.3905 11.00000 0.05 1.44 Q8 1 0.6939 0.4103 0.4235 11.00000 0.05 1.42 Q9 1 0.7646 0.6538 0.3588 11.00000 0.05 1.27 Q10 1 0.6621 0.5002 0.3208 11.00000 0.05 1.22 ; _shelx_res_checksum 47570 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