data_11 _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common 'nioboheftetjernite' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Fe0.37 Mn0.08 Nb0.58 O4 Sc0.40 Ta0.41 Ti0.16' _chemical_formula_weight 242.79 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' 'Nb' 'Nb' -2.0727 0.6215 '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sc' 'Sc' 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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/c' _space_group_name_Hall '-P 2yc' _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+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 4.7092(3) _cell_length_b 5.6531(4) _cell_length_c 5.0530(4) _cell_angle_alpha 90 _cell_angle_beta 90.453(3) _cell_angle_gamma 90 _cell_volume 134.515(17) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4930 _cell_measurement_theta_min 3.604 _cell_measurement_theta_max 40.191 _exptl_crystal_description anhedral _exptl_crystal_colour black _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 5.994 _exptl_crystal_F_000 219 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_absorpt_coefficient_mu 22.778 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5961 _exptl_absorpt_correction_T_max 0.7479 _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10. ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Incoatec Microfocus Source IµS' _diffrn_measurement_device_type 'Bruker Kappa X8 APEX' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7860 _diffrn_reflns_av_unetI/netI 0.0128 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.604 _diffrn_reflns_theta_max 40.308 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.971 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_Laue_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_point_group_measured_fraction_full 0.971 _reflns_number_total 847 _reflns_number_gt 814 _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 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _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^)+(0.0116P)^2^+0.6361P] 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 847 _refine_ls_number_parameters 29 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0173 _refine_ls_R_factor_gt 0.0158 _refine_ls_wR_factor_ref 0.0359 _refine_ls_wR_factor_gt 0.0355 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Nb Nb 0.500000 0.32276(3) 0.250000 0.00626(4) Uani 0.58 2 d S T P . . Ta1 Ta 0.500000 0.32276(3) 0.250000 0.00626(4) Uani 0.34 2 d S T P . . Ti1 Ti 0.500000 0.32276(3) 0.250000 0.00626(4) Uani 0.08 2 d S T P . . Sc Sc 0.000000 0.82766(6) 0.250000 0.00749(5) Uani 0.4 2 d S T P . . Fe Fe 0.000000 0.82766(6) 0.250000 0.00749(5) Uani 0.37 2 d S T P . . Ta2 Ta 0.000000 0.82766(6) 0.250000 0.00749(5) Uani 0.07 2 d S T P . . Ti2 Ti 0.000000 0.82766(6) 0.250000 0.00749(5) Uani 0.08 2 d S T P . . Mn Mn 0.000000 0.82766(6) 0.250000 0.00749(5) Uani 0.08 2 d S T P . . O1 O 0.2767(3) 0.6110(3) 0.0719(3) 0.0105(2) Uani 1 1 d . . . . . O2 O 0.2345(3) 0.1164(2) 0.0893(3) 0.0094(2) 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 Nb 0.00691(6) 0.00529(6) 0.00658(6) 0.000 -0.00134(4) 0.000 Ta1 0.00691(6) 0.00529(6) 0.00658(6) 0.000 -0.00134(4) 0.000 Ti1 0.00691(6) 0.00529(6) 0.00658(6) 0.000 -0.00134(4) 0.000 Sc 0.00732(12) 0.00809(12) 0.00706(12) 0.000 0.00037(9) 0.000 Fe 0.00732(12) 0.00809(12) 0.00706(12) 0.000 0.00037(9) 0.000 Ta2 0.00732(12) 0.00809(12) 0.00706(12) 0.000 0.00037(9) 0.000 Ti2 0.00732(12) 0.00809(12) 0.00706(12) 0.000 0.00037(9) 0.000 Mn 0.00732(12) 0.00809(12) 0.00706(12) 0.000 0.00037(9) 0.000 O1 0.0116(5) 0.0096(5) 0.0104(5) 0.0031(4) -0.0016(4) -0.0010(4) O2 0.0092(5) 0.0086(5) 0.0106(5) -0.0006(4) 0.0000(4) -0.0016(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 Nb O2 1.8885(14) . ? Nb O2 1.8885(14) 2_655 ? Nb O1 1.9796(15) 4_566 ? Nb O1 1.9796(15) 3_665 ? Nb O1 2.1346(14) 2_655 ? Nb O1 2.1346(14) . ? Nb Nb 3.2247(3) 3_666 ? Nb Nb 3.2247(3) 3_665 ? Sc O1 2.0064(16) 2 ? Sc O1 2.0064(16) . ? Sc O2 2.0565(14) 4_566 ? Sc O2 2.0565(14) 3_565 ? Sc O2 2.1351(14) 1_565 ? Sc O2 2.1351(14) 2_565 ? Sc Sc 3.1906(5) 3_576 ? Sc Sc 3.1906(5) 3_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb O2 103.72(9) . 2_655 ? O2 Nb O1 96.66(6) . 4_566 ? O2 Nb O1 96.75(6) 2_655 4_566 ? O2 Nb O1 96.75(6) . 3_665 ? O2 Nb O1 96.66(6) 2_655 3_665 ? O1 Nb O1 158.21(9) 4_566 3_665 ? O2 Nb O1 167.16(6) . 2_655 ? O2 Nb O1 88.17(6) 2_655 2_655 ? O1 Nb O1 76.85(7) 4_566 2_655 ? O1 Nb O1 86.50(5) 3_665 2_655 ? O2 Nb O1 88.17(6) . . ? O2 Nb O1 167.16(6) 2_655 . ? O1 Nb O1 86.50(5) 4_566 . ? O1 Nb O1 76.85(7) 3_665 . ? O1 Nb O1 80.46(8) 2_655 . ? O2 Nb Nb 135.77(4) . 3_666 ? O2 Nb Nb 92.92(4) 2_655 3_666 ? O1 Nb Nb 40.14(4) 4_566 3_666 ? O1 Nb Nb 121.98(4) 3_665 3_666 ? O1 Nb Nb 36.71(4) 2_655 3_666 ? O1 Nb Nb 81.54(4) . 3_666 ? O2 Nb Nb 92.92(4) . 3_665 ? O2 Nb Nb 135.77(4) 2_655 3_665 ? O1 Nb Nb 121.98(4) 4_566 3_665 ? O1 Nb Nb 40.14(4) 3_665 3_665 ? O1 Nb Nb 81.54(4) 2_655 3_665 ? O1 Nb Nb 36.71(4) . 3_665 ? Nb Nb Nb 103.161(10) 3_666 3_665 ? O1 Sc O1 104.77(8) 2 . ? O1 Sc O2 93.80(6) 2 4_566 ? O1 Sc O2 96.96(6) . 4_566 ? O1 Sc O2 96.96(6) 2 3_565 ? O1 Sc O2 93.80(6) . 3_565 ? O2 Sc O2 162.33(8) 4_566 3_565 ? O1 Sc O2 167.68(6) 2 1_565 ? O1 Sc O2 87.50(6) . 1_565 ? O2 Sc O2 85.62(5) 4_566 1_565 ? O2 Sc O2 80.88(6) 3_565 1_565 ? O1 Sc O2 87.50(6) 2 2_565 ? O1 Sc O2 167.68(6) . 2_565 ? O2 Sc O2 80.88(6) 4_566 2_565 ? O2 Sc O2 85.62(5) 3_565 2_565 ? O2 Sc O2 80.26(8) 1_565 2_565 ? O1 Sc Sc 90.77(4) 2 3_576 ? O1 Sc Sc 137.05(4) . 3_576 ? O2 Sc Sc 41.36(4) 4_566 3_576 ? O2 Sc Sc 124.26(4) 3_565 3_576 ? O2 Sc Sc 80.65(4) 1_565 3_576 ? O2 Sc Sc 39.52(4) 2_565 3_576 ? O1 Sc Sc 137.05(4) 2 3_575 ? O1 Sc Sc 90.77(4) . 3_575 ? O2 Sc Sc 124.26(4) 4_566 3_575 ? O2 Sc Sc 41.36(4) 3_565 3_575 ? O2 Sc Sc 39.52(4) 1_565 3_575 ? O2 Sc Sc 80.65(4) 2_565 3_575 ? Sc Sc Sc 104.72(2) 3_576 3_575 ? O1 Sc Ti1 75.11(4) 2 3_565 ? O1 Sc Ti1 87.94(4) . 3_565 ? O2 Sc Ti1 168.74(4) 4_566 3_565 ? O2 Sc Ti1 24.90(4) 3_565 3_565 ? O2 Sc Ti1 104.78(4) 1_565 3_565 ? O2 Sc Ti1 96.42(4) 2_565 3_565 ? Sc Sc Ti1 134.991(8) 3_576 3_565 ? Sc Sc Ti1 65.551(5) 3_575 3_565 ? Nb O1 Sc 127.17(7) 3_665 . ? Nb O1 Nb 103.15(7) 3_665 . ? Sc O1 Nb 126.61(7) . . ? Nb O2 Sc 127.80(7) . 3_565 ? Nb O2 Sc 130.64(8) . 1_545 ? Sc O2 Sc 99.12(6) 3_565 1_545 ? _refine_diff_density_max 1.361 _refine_diff_density_min -1.415 _refine_diff_density_rms 0.213