data_stibiotantalite _audit_creation_date 2022-10-26 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number '2018/3' _chemical_name_common 'stibiotantalite' _chemical_formula_moiety 'Nb0.211 O4 Sb Ta0.789' _chemical_formula_sum 'Nb0.21 O4 Sb Ta0.79' _chemical_formula_weight 347.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Nb' 'Nb' -2.0727 0.6215 '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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ta' 'Ta' -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'orthorhombic' _space_group_IT_number 33 _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' loop_ _space_group_symop_operation_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 5.5419(2) _cell_length_b 4.9200(2) _cell_length_c 11.8003(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 321.75(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2042 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.293 _cell_measurement_theta_min 3.42 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 35.742 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 7.184 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description granular _exptl_crystal_F_000 597 _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_unetI/netI 0.0191 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.925 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 2558 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.871 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 29.394 _diffrn_reflns_theta_min 3.453 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.925 _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single' _diffrn_measurement_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.802 _reflns_Friedel_fraction_full 0.978 _reflns_Friedel_fraction_max 0.812 _reflns_number_gt 766 _reflns_number_total 775 _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. Completness statistics refer to single and composite reflections containing twin component 1 only. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 1.378 _refine_diff_density_min -0.971 _refine_diff_density_rms 0.240 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.38(3) _refine_ls_extinction_coef 0.0013(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 58 _refine_ls_number_reflns 775 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0175 _refine_ls_R_factor_gt 0.0173 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.1990P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0436 _refine_special_details ; Refined as a 2-component inversion twin. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.62(3) 0.38(3) 2. Shared sites {Ta, Nb} 3. Uiso/Uaniso restraints and constraints Uanis(Ta) = Uanis(Nb) 4. Others Sof(Nb)=1-FVAR(1) Sof(Ta)=FVAR(1) ; _atom_sites_solution_hydrogens . _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 Sb Sb 0.52197(13) 0.95378(10) 0.60230(9) 0.00915(19) Uani 1 1 d . . . A 2 Ta Ta 0.61710(7) 0.50553(7) 0.35081(13) 0.00483(16) Uani 0.789(5) 1 d . . P A . Nb Nb 0.61710(7) 0.50553(7) 0.35081(13) 0.00483(16) Uani 0.211(5) 1 d . . P A . O1 O 0.4149(12) 0.7863(12) 0.2933(6) 0.0114(13) Uani 1 1 d . . . . . O2 O 0.3718(9) 0.2709(11) 0.3976(6) 0.0094(13) Uani 1 1 d . . . . . O3 O 0.6751(10) 0.6647(13) 0.5029(7) 0.0098(13) Uani 1 1 d . . . . . O4 O 0.3454(10) 0.6671(13) 0.6928(6) 0.0092(13) 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 Sb 0.0075(3) 0.0099(3) 0.0100(3) 0.0012(8) 0.0015(4) 0.0001(2) Ta 0.0029(2) 0.0058(2) 0.0058(2) -0.00006(14) -0.00017(19) 0.00002(10) Nb 0.0029(2) 0.0058(2) 0.0058(2) -0.00006(14) -0.00017(19) 0.00002(10) O1 0.012(3) 0.008(3) 0.014(4) -0.001(3) 0.001(2) -0.001(2) O2 0.014(3) 0.007(3) 0.007(4) 0.001(3) 0.001(2) -0.003(2) O3 0.010(3) 0.006(3) 0.013(4) -0.003(2) -0.002(2) 0.001(3) O4 0.007(3) 0.016(3) 0.005(4) 0.002(3) -0.001(2) -0.002(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 Sb O1 2.615(7) 2_675 ? Sb O2 2.993(7) 1_565 ? Sb O3 2.030(7) . ? Sb O3 2.326(6) 3_465 ? Sb O4 2.022(7) . ? Sb O4 2.170(6) 3_565 ? Ta O1 2.057(6) 3_565 ? Ta O1 1.904(6) . ? Ta O2 1.867(5) . ? Ta O2 2.037(5) 3 ? Ta O3 1.984(8) . ? Ta O4 2.059(7) 2_664 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sb O2 118.53(16) 2_675 1_565 ? O3 Sb O1 131.9(2) 3_465 2_675 ? O3 Sb O1 141.7(2) . 2_675 ? O3 Sb O2 90.9(3) . 1_565 ? O3 Sb O2 59.6(2) 3_465 1_565 ? O3 Sb O3 83.0(2) . 3_465 ? O3 Sb O4 75.3(2) . 3_565 ? O4 Sb O1 87.2(3) . 2_675 ? O4 Sb O1 66.4(2) 3_565 2_675 ? O4 Sb O2 131.0(2) . 1_565 ? O4 Sb O2 140.3(2) 3_565 1_565 ? O4 Sb O3 72.1(2) . 3_465 ? O4 Sb O3 149.57(19) 3_565 3_465 ? O4 Sb O3 91.1(2) . . ? O4 Sb O4 87.0(2) . 3_565 ? Sb Ta Sb 54.58(3) 3_565 . ? Sb Ta Sb 140.925(15) 4_644 . ? O1 Ta Sb 95.1(2) . 4_644 ? O1 Ta Sb 94.7(2) 3_565 . ? O1 Ta Sb 101.8(2) 3_565 2_664 ? O1 Ta Sb 46.6(2) 3_565 4_644 ? O1 Ta Sb 92.1(2) . 2_664 ? O1 Ta Sb 126.8(2) . 3_565 ? O1 Ta Sb 76.8(2) . . ? O1 Ta Sb 75.7(2) 3_565 3_565 ? O1 Ta O1 89.62(16) . 3_565 ? O1 Ta O2 171.6(3) . 3 ? O1 Ta O3 97.5(3) . . ? O1 Ta O4 80.0(3) 3_565 2_664 ? O1 Ta O4 92.1(3) . 2_664 ? O2 Ta Sb 91.6(2) . . ? O2 Ta Sb 77.7(2) 3 4_644 ? O2 Ta Sb 53.3(2) 3 3_565 ? O2 Ta Sb 127.5(2) . 4_644 ? O2 Ta Sb 106.1(2) 3 . ? O2 Ta Sb 73.2(2) . 2_664 ? O2 Ta Sb 103.6(2) . 3_565 ? O2 Ta Sb 87.3(2) 3 2_664 ? O2 Ta O1 171.7(3) . 3_565 ? O2 Ta O1 97.2(3) . . ? O2 Ta O1 82.3(2) 3 3_565 ? O2 Ta O2 90.66(14) . 3 ? O2 Ta O3 95.4(3) . . ? O2 Ta O4 84.3(3) 3 2_664 ? O2 Ta O4 95.0(3) . 2_664 ? O3 Ta Sb 133.03(17) . 4_644 ? O3 Ta Sb 166.0(2) . 2_664 ? O3 Ta Sb 32.95(16) . 3_565 ? O3 Ta Sb 21.75(16) . . ? O3 Ta O1 88.4(3) . 3_565 ? O3 Ta O2 84.6(3) . 3 ? O3 Ta O4 164.9(2) . 2_664 ? O4 Ta Sb 33.67(16) 2_664 4_644 ? O4 Ta Sb 21.87(16) 2_664 2_664 ? O4 Ta Sb 133.04(17) 2_664 3_565 ? O4 Ta Sb 167.74(19) 2_664 . ? Ta O1 Sb 125.7(3) . 2_674 ? Ta O1 Sb 98.5(2) 3_465 2_674 ? Ta O1 Ta 135.7(4) . 3_465 ? Ta O2 Sb 111.0(3) . 1_545 ? Ta O2 Sb 93.6(2) 3_455 1_545 ? Ta O2 Ta 146.8(4) . 3_455 ? Ta O3 Sb 119.4(3) . 3_565 ? Ta O3 Sb 137.0(3) . . ? Ta O4 Sb 114.6(3) 2_665 3_465 ? 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 Sb Ta O2 Sb -71.0(2) . . . 1_545 ? Sb Ta O2 Sb -17.2(2) 3_565 . . 1_545 ? Sb Ta O2 Sb 110.0(3) 4_644 . . 1_545 ? Sb Ta O2 Sb 122.0(2) 2_664 . . 1_545 ? Sb Ta O2 Ta -152.6(5) 3_565 . . 3_455 ? Sb Ta O2 Ta -25.5(7) 4_644 . . 3_455 ? Sb Ta O2 Ta 153.5(5) . . . 3_455 ? Sb Ta O2 Ta -13.4(5) 2_664 . . 3_455 ? O1 Ta O2 Sb -147.9(2) . . . 1_545 ? O1 Ta O2 Ta 76.7(6) . . . 3_455 ? O2 Ta O2 Sb 35.1(4) 3 . . 1_545 ? O2 Ta O2 Ta -100.4(7) 3 . . 3_455 ? O3 Ta O2 Sb -49.6(3) . . . 1_545 ? O3 Ta O2 Ta 175.0(5) . . . 3_455 ? O4 Ta O2 Sb 119.4(3) 2_664 . . 1_545 ? O4 Ta O2 Ta -16.1(6) 2_664 . . 3_455 ? loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l _diffrn_refln_intensity_net _diffrn_refln_intensity_u 0 0 -15 -0.21 2.4 0 0 -14 227.63 11.06 0 0 -13 1.24 2.1 0 0 -12 3817.56 68.04 0 0 -11 -0.44 1.54 0 0 -10 39.06 3.78 0 0 -9 1.56 0.54 0 0 -9 1.41 1.33 0 0 -8 6434.91 95.23 0 0 -8 6167.36 101.72 0 0 -7 0.91 1.4 0 0 -7 1.42 0.55 0 0 -6 488.33 12.13 0 0 -6 494.47 12.25 0 0 -5 2.35 0.86 0 0 -5 11.25 1.66 0 0 -4 9407.02 142.42 0 0 -4 9443.09 142.02 0 0 -3 1.14 0.9 0 0 -3 1.39 0.64 0 0 -2 565.01 10.34 0 0 2 537.09 9.84 0 0 2 545.44 10.04 0 0 3 1.52 0.73 0 0 3 1.6 0.87 0 0 4 9999 148.04 0 0 4 9623.88 147.71 0 0 5 0.29 1.16 0 0 5 6.5 1.31 0 0 6 512.55 12.96 0 0 6 490.95 12.07 0 0 6 505.44 13.78 0 0 7 2.57 1.53 0 0 8 6654.73 106.37 0 1 -15 12.61 3.41 0 -1 -14 0.62 2.31 0 1 -14 0.18 2.09 0 -1 -13 101.8 7.35 0 1 -13 91.53 6.32 0 1 -12 -0.07 1.75 0 -1 -12 1.72 2.04 0 1 -11 93.9 5.79 0 -1 -11 90.78 6.35 0 -1 -10 1.18 1.63 0 1 -10 1.38 1.16 0 1 -10 0.42 1.35 0 1 -9 118.6 6.05 0 -1 -9 119.59 6.63 0 1 -8 0.53 0.98 0 1 -8 0.98 1.47 0 1 -8 0.98 1.11 0 1 -7 169.5 6.38 0 1 -7 167.36 6.32 0 1 -6 1.51 0.88 0 1 -6 2.55 0.97 0 1 -6 0.4 1.07 0 1 -5 76.18 3.41 0 -1 -5 71.91 4.31 0 1 -5 75.21 3.33 0 -1 -4 0.67 0.69 0 1 -4 0.78 0.59 0 -1 -3 535.54 11.35 0 1 -3 514.48 9.58 0 1 -2 1.66 0.42 0 -1 -2 0.73 0.53 0 -1 -2 0.73 0.61 0 -1 -2 1.15 0.63 0 -1 -1 436.1 8.3 0 1 -1 441.62 7.94 0 -1 0 0.96 0.32 0 1 0 0.86 0.37 0 -1 0 0.43 0.35 0 -1 0 1.08 0.36 0 1 1 483.1 8.93 0 1 1 458.04 8.54 0 -1 1 466.2 7.93 0 1 2 1.23 0.73 0 1 2 0.8 0.56 0 1 3 508.71 9.37 0 1 3 503.37 11.03 0 1 3 499.74 10.74 0 -1 4 0.22 0.59 0 1 4 0.07 0.93 0 1 4 0.72 0.89 0 1 4 0.94 0.51 0 1 5 75.6 4.21 0 -1 5 70.09 3.12 0 1 5 65.75 2.25 0 1 5 72.17 4.26 0 1 6 0.61 1.12 0 -1 6 1.68 0.97 0 1 7 171.2 7.41 0 -1 7 151.58 5.79 0 1 8 1.14 1.63 0 1 9 121.75 6.87 0 1 10 2.23 2.27 0 1 11 100.87 6.8 0 1 12 2.22 2.6 0 2 -15 0.36 2.32 0 2 -14 231.1 10.34 0 2 -13 0.82 1.87 0 2 -12 2947.28 53.28 0 -2 -11 2.55 2.07 0 2 -11 0.06 1.55 0 -2 -10 631.16 18.97 0 2 -10 649.63 16.42 0 2 -9 2.61 1.47 0 2 -9 6.68 1.93 0 -2 -8 5466.26 90.75 0 2 -8 5525.78 86.31 0 2 -8 5354.65 85.82 0 -2 -7 7.29 2.06 0 2 -7 0.29 1.2 0 2 -7 9.55 1.75 0 -2 -7 0.76 1.29 0 2 -7 0.63 0.93 0 -2 -6 433.98 12.77 0 2 -6 472.14 12.41 0 2 -6 441.46 10.33 0 -2 -6 452.01 13.18 0 -2 -5 2.51 1.19 0 2 -5 1.32 0.77 0 -2 -5 1.51 1.09 0 2 -5 3.47 1.39 0 2 -4 7441.07 112.71 0 2 -4 7676.05 116.65 0 -2 -4 7305.09 116.22 0 -2 -4 7676.53 115.91 0 2 -3 7.58 0.78 0 -2 -3 7.2 1.29 0 -2 -3 7.65 1.39 0 -2 -2 284.38 7.51 0 2 -2 290.28 8.41 0 2 -2 275.03 6.89 0 -2 -2 276.84 7.49 0 2 -1 10.95 1.17 0 2 -1 11.15 1.03 0 2 -1 9.21 0.8 0 2 -1 10.97 1.36 0 -2 0 5910.02 91.13 0 2 0 6017.09 92.65 0 -2 0 5786.72 90.24 0 2 0 5947.62 89.7 0 2 0 6029.14 91.15 0 -2 0 6115.54 90.23 0 2 0 5919.39 90.09 0 2 1 0.68 0.87 0 -2 1 7.45 0.92 0 2 1 2.93 0.81 0 2 1 1.65 0.81 0 -2 1 6.89 1.09 0 2 1 1.26 0.71 0 2 2 292.28 7.35 0 -2 2 282.1 6.44 0 2 2 299.66 7.65 0 -2 2 279.96 7.49 0 2 2 304.86 8.02 0 -2 2 278.89 6.68 0 2 2 289.5 7.53 0 -2 3 6.3 1.06 0 2 3 3.47 1.1 0 2 3 1.09 0.89 0 -2 3 5.08 1.09 0 2 3 1.66 0.97 0 -2 4 7153.82 113.82 0 2 4 7472.35 114.64 0 2 4 7423.02 112.7 0 2 4 7625 114.61 0 -2 5 3.4 1.18 0 2 5 2.65 1.36 0 2 6 408.69 9.2 0 2 7 0.44 1.51 0 2 7 8.05 1.15 0 2 8 5648.52 93.85 0 2 9 23.78 3.47 0 2 10 644.59 18.75 0 2 11 13.28 3.13 0 2 12 3179.05 60.48 0 2 13 1.64 2.68 0 2 14 236.32 11.78 0 -3 -12 1.09 2.32 0 3 -11 340.88 10.92 0 -3 -11 352.15 14.22 0 3 -10 0.34 1.34 0 -3 -10 1.07 1.85 0 -3 -9 355.61 13.22 0 3 -9 401.04 10.85 0 -3 -8 1.95 1.83 0 3 -8 1.17 1.15 0 3 -8 0.55 1.29 0 -3 -8 2.1 1.71 0 -3 -7 383.91 12.85 0 -3 -7 383.84 12.92 0 3 -7 381.65 9.33 0 3 -6 0.79 0.83 0 -3 -6 0.7 1.32 0 -3 -6 0.18 1.32 0 -3 -5 885.89 19.92 0 -3 -5 880.02 20.29 0 3 -5 905.6 16.05 0 -3 -4 1.25 1.18 0 -3 -4 1.2 1.14 0 -3 -4 0.58 1.01 0 3 -4 1.86 0.66 0 -3 -3 481.01 11.94 0 -3 -3 510.27 12.75 0 3 -2 0.51 0.61 0 3 -2 2.26 1.09 0 -3 -2 2.77 1.07 0 -3 -2 0.8 0.92 0 3 -1 992.91 16.58 0 3 -1 898.58 17.65 0 3 -1 948.61 17.06 0 -3 -1 856.52 17.83 0 -3 -1 923.16 19.06 0 3 0 0.43 0.68 0 3 0 0.19 0.71 0 -3 0 0.34 0.77 0 3 1 992.44 18.09 0 3 1 900.48 17.94 0 -3 1 963.5 17.8 0 -3 1 916.64 19.1 0 3 2 1.29 1.02 0 -3 2 1.2 0.74 0 3 2 2.32 1.04 0 -3 2 3.13 1.09 0 -3 3 503.81 11.22 0 3 3 508.13 12.74 0 -3 3 488.23 12.42 0 3 3 492.31 12.14 0 3 3 506.35 12.34 0 -3 4 4.32 1.29 0 3 4 2 1.19 0 -3 4 0.71 0.95 0 -3 4 3.16 0.98 0 3 5 889.05 20.4 0 3 5 890.05 18.27 0 -3 5 883.31 19.48 0 -3 5 863.38 17.88 0 -3 5 825.89 17.24 0 -3 6 2.41 1.24 0 3 6 1.01 1.04 0 -3 6 1.98 1.36 0 3 6 3.88 1.75 0 3 7 331.08 9.03 0 -3 7 345.04 10.66 0 3 7 355.56 12.34 0 -3 8 0.06 1.45 0 -3 9 381.04 12.95 0 -3 10 0.64 1.96 0 3 10 0.27 2.12 0 3 11 343.5 13.62 0 -3 11 290.63 12.53 0 3 12 0.9 2.63 0 -3 12 0.3 2.34 0 -3 13 140.08 9.24 0 -3 14 0.36 3.07 0 -4 -11 1.08 2.41 0 -4 -10 562.31 18.6 0 -4 -9 1.12 2.09 0 -4 -8 1824.22 37.97 0 -4 -8 1753.23 37.75 0 -4 -7 16.33 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12.14 5 -3 -1 428.72 13.29 5 3 -1 394.89 14.47 5 -3 -1 418.67 11.76 -5 -3 -1 399.18 18.21 5 -3 -1 408.61 14.67 5 -3 0 2147.72 40.46 5 -3 0 2090.43 37.83 5 3 0 2156.64 44.6 5 -3 0 2143.48 43.71 5 -3 1 478.33 13.71 5 3 1 442.69 15.89 5 -3 1 449.77 15.54 5 -3 2 431.54 13.04 5 3 2 423.64 15.38 -5 -3 2 391.93 18.1 5 -3 2 436.46 15.25 5 -3 3 616.21 18.78 5 -3 3 627.76 16.38 5 -3 4 1614.33 36 5 -3 4 1697.5 32.88 5 -3 5 345.77 11.79 5 -3 5 368.59 14.33 5 -3 6 400.39 13.2 5 -3 6 394.94 15.23 -5 -3 7 241.37 12.94 5 -3 7 270.98 10.83 -5 -3 8 1158.9 32.3 5 -3 8 1337.22 29.38 -5 -3 9 255.98 12.88 5 -3 9 311 12.28 5 -3 10 238.36 11.14 -5 -4 -5 141.25 10.91 -5 -4 -4 171.51 12.06 5 -4 -3 213.41 10.31 -5 -4 -3 215.36 13.73 5 -4 -2 109.13 7.19 5 4 -2 115.39 7.98 -5 -4 -2 95.9 9.45 5 -4 -1 265.94 11.28 5 4 -1 261.29 12.17 -5 -4 -1 243.05 14.72 5 -4 0 219.73 9.92 5 4 0 213.82 10.99 -5 -4 0 202.81 13.36 5 -4 1 270.53 11.05 5 4 1 278.4 12.89 5 -4 2 117.66 7.04 5 4 2 118.24 8.44 -5 -4 2 94.52 9.38 5 4 3 222.25 11.54 -5 -4 3 210.74 13.72 5 -4 3 245.16 10.55 5 -4 4 176.73 8.67 5 -4 5 144.3 7.9 5 -4 6 75.04 5.99 5 -4 7 164.89 9.02 -6 0 -8 31.73 5.49 6 0 -7 1020.1 27.05 -6 0 -7 1186.37 32.16 6 0 -6 394.46 13.46 -6 0 -6 451.55 18.46 -6 0 -5 1496.73 38.39 -6 0 -4 26.72 4.94 -6 0 -3 1295.66 35.03 -6 0 -1 1564.73 39.53 6 0 -1 1546.37 31.76 -6 0 0 47.56 6.15 6 0 0 48.58 4.34 6 0 0 53 4.43 -6 0 1 1488 38.74 6 0 1 1534.51 31.44 6 0 1 1599.68 32.46 6 0 2 892.35 21.56 -6 0 2 848.91 27.02 6 0 2 880.65 21.52 6 0 3 1416.12 29.82 6 0 3 1400 30.13 6 0 4 16.77 3.11 -6 0 4 17.78 4.31 -6 0 5 1463.59 37.2 6 0 5 1542.6 33.38 -6 0 6 429.58 17.39 6 0 6 432.15 15 -6 0 7 1086.32 29.75 6 0 7 1202.71 29.11 6 0 8 30.54 4.68 6 -1 -9 20.74 4.25 6 -1 -8 11.45 3.3 -6 -1 -8 17.75 4.69 -6 1 -7 6.22 3.65 -6 -1 -7 4.93 3.44 6 -1 -7 3.68 2.58 6 -1 -6 21.76 3.71 -6 1 -6 20.9 4.81 -6 -1 -6 21.9 4.76 -6 1 -5 6.91 3.65 -6 -1 -5 7.55 3.51 -6 1 -4 7.04 3.59 -6 -1 -4 3.82 3.15 -6 -1 -3 6.55 3.37 -6 1 -2 66.29 7.3 -6 1 -1 61.74 7.02 6 1 -1 61.87 5.25 6 -1 -1 61.71 5.15 6 -1 0 10.12 2.52 6 1 0 10.87 2.82 -6 1 0 8.51 3.65 -6 -1 0 8.91 3.73 -6 1 1 60.64 6.89 6 1 1 68.23 5.7 -6 -1 1 60.41 7.03 6 -1 1 63.83 4.19 6 -1 1 67.85 5.54 6 1 1 64.62 4.36 6 1 2 73.82 5.81 -6 1 2 61.83 6.94 -6 -1 2 65.26 7.38 6 -1 2 69.05 4.39 6 1 2 63.83 4.48 6 -1 2 69.5 5.55 6 1 3 7.64 2.2 6 -1 3 8.24 2.56 6 1 3 9.95 2.85 6 -1 3 10.22 2.26 -6 1 3 6.85 3.38 -6 -1 3 8.11 3.48 6 1 4 4.94 2.05 6 -1 4 4.17 2.33 6 -1 4 4.91 2.01 -6 1 4 6.66 3.33 -6 -1 4 3.14 2.87 6 1 5 8.4 2.48 6 -1 5 9.14 2.91 -6 1 5 7.56 3.26 -6 -1 5 8.75 3.46 -6 1 6 18.54 4.25 -6 -1 6 22.09 4.58 6 1 6 23.2 3.71 6 -1 6 25.32 4.19 6 1 7 3.9 2.45 6 -1 7 5.92 2.86 -6 1 7 5.75 2.99 -6 -1 7 4.51 2.89 6 1 8 13.76 3.55 -6 -1 8 14.52 3.77 6 1 9 22.2 4.28 -6 -2 -7 975.54 29.13 6 -2 -7 875.04 23.92 -6 -2 -6 563.22 21.37 6 -2 -6 495.82 16.31 -6 -2 -5 1207.31 34.21 6 -2 -5 1169.03 27.46 6 -2 -4 18.98 3.44 -6 -2 -4 18.62 4.7 6 -2 -3 1294.6 28.63 -6 -2 -3 1265.17 35.99 -6 -2 -2 432.58 19.23 6 2 -2 435.61 15.48 6 2 -1 1403.1 32.24 6 -2 -1 1418.36 32.71 6 -2 0 9.9 3.04 6 2 0 2.39 2.62 -6 -2 0 14.44 4.19 -6 2 1 1416.03 37.95 6 2 1 1534.25 34.21 6 -2 1 1467.45 33.26 -6 2 2 471.27 19.39 6 2 2 477.75 16.53 -6 -2 2 421.21 19.12 6 -2 2 467.53 16.2 6 2 3 1459.77 33.27 -6 2 3 1397.58 37.21 6 -2 3 1415.11 32.75 6 -2 4 17.53 3.62 -6 2 4 17.51 4.45 -6 -2 4 18.12 4.6 -6 2 5 1260.21 33.27 6 -2 5 1268.33 31.04 -6 2 6 514.54 19.3 -6 -2 6 500.25 20.12 6 -2 6 541.58 18.56 -6 -2 7 891.21 27.16 -6 -2 8 5.7 3.42 6 -3 -6 173.05 9.19 6 -3 -5 67.52 5.81 6 -3 -4 55.14 5.1 6 3 -1 96.89 7.52 6 -3 -1 92.08 7.34 6 3 0 87.88 7.19 6 -3 0 85.03 6.99 6 3 1 103.11 8.09 6 -3 1 99.27 7.5 6 -3 2 175.06 10.09 -6 3 5 74.89 7.97 7 0 1 1.72 2.26 7 0 2 0.73 2.33 7 0 3 0.74 2.22 7 0 3 0.86 2.41 -7 0 3 -0.61 3.49 7 0 4 0.59 2.24 7 0 4 1.44 2.62 -7 0 4 -0.74 3.41 7 0 5 0.55 2.27 7 0 6 2.41 2.64 7 1 0 28.46 4.24 7 -1 0 24.87 4.15 7 1 1 1102.94 27.47 7 -1 1 1111.6 27.5 7 1 2 621.51 19.16 7 -1 2 629.33 19.4 7 1 3 1284.81 30.72 7 -1 3 1199.12 29.92 7 1 4 14.39 3.86 7 -1 4 26.2 4.35 7 -2 -3 26.83 4.2 _iucr_refine_instructions_details ; TITL 2019005a_e.res in Pna2(1) 2019005a-stibi.res created by SHELXL-2018/3 at 21:07:08 on 26-Oct-2022 CELL 0.71073 5.5419 4.92 11.8003 90 90 90 ZERR 4 0.0002 0.0002 0.0005 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,+Z SYMM 0.5-X,0.5+Y,0.5+Z SFAC Nb O Sb Ta UNIT 0.85 16 4 3.15 EADP Ta Nb EXYZ Ta Nb L.S. 20 PLAN 5 CONF CONN 6 2 Sb MORE -1 fmap 2 acta 50 TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.025700 0.199000 EXTI 0.001263 BASF 0.38362 FVAR 0.28401 0.78857 PART 2 SB 3 0.521966 0.953783 0.602298 11.00000 0.00751 0.00992 = 0.01003 0.00118 0.00150 0.00007 PART 0 TA 4 0.617096 0.505530 0.350814 21.00000 0.00292 0.00577 = 0.00581 -0.00006 -0.00017 0.00002 NB 1 0.617096 0.505530 0.350814 -21.00000 0.00292 0.00577 = 0.00581 -0.00006 -0.00017 0.00002 O1 2 0.414884 0.786283 0.293309 11.00000 0.01214 0.00772 = 0.01426 -0.00142 0.00091 -0.00073 O2 2 0.371840 0.270944 0.397642 11.00000 0.01364 0.00748 = 0.00712 0.00080 0.00059 -0.00344 O3 2 0.675137 0.664722 0.502873 11.00000 0.01048 0.00569 = 0.01323 -0.00316 -0.00225 0.00083 O4 2 0.345434 0.667098 0.692831 11.00000 0.00658 0.01578 = 0.00515 0.00243 -0.00084 -0.00170 HKLF 4 REM 2019005a_e.res in Pna2(1) REM wR2 = 0.0436, GooF = S = 1.158, Restrained GooF = 1.157 for all data REM R1 = 0.0173 for 766 Fo > 4sig(Fo) and 0.0175 for all 775 data REM 58 parameters refined using 1 restraints END WGHT 0.0257 0.1992 REM Highest difference peak 1.378, deepest hole -0.971, 1-sigma level 0.240 Q1 1 0.4917 0.6258 0.3436 11.00000 0.05 1.38 Q2 1 0.5081 0.3780 0.3604 11.00000 0.05 1.37 Q3 1 0.5024 1.0991 0.6017 11.00000 0.05 1.16 Q4 1 0.7525 0.5975 0.3485 11.00000 0.05 1.07 Q5 1 0.7378 0.3842 0.3543 11.00000 0.05 0.99 REM The information below was added by Olex2. REM REM R1 = 0.0173 for 766 Fo > 4sig(Fo) and 0.0175 for all 2922 data REM 58 parameters refined using n/a restraints REM Highest difference peak 1.38, deepest hole -0.97 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0175 REM R1_gt = 0.0173 REM wR_ref = 0.0436 REM GOOF = 1.158 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 2922 REM Reflections_gt = 766 REM Parameters = 58 REM Hole = -0.97 REM Peak = 1.38 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.62(3) 2 0.38(3)