# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1191 data_okay _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'O5 S2 Sm2 Ti2' _chemical_formula_weight 540.62 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 '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' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 3.8180(10) _cell_length_b 3.8180(10) _cell_length_c 22.952(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 334.57(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 35 _exptl_crystal_description rod _exptl_crystal_colour brown-yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.366 _exptl_crystal_density_method ? _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 20.173 _exptl_absorpt_correction_type 'semi-empirical from psi-scans' _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.78 _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 'P21 four circle diffractometer' _diffrn_measurement_method theta-2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1066 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0142 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 5.41 _diffrn_reflns_theta_max 26.94 _reflns_number_total 129 _reflns_number_observed 127 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'P21 data collection programs' _computing_cell_refinement 'P21 data collection programs' _computing_data_reduction 'SHELXTL (Siemens, 1986)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Diamond' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+0.3337P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0081(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 129 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0145 _refine_ls_R_factor_obs 0.0142 _refine_ls_wR_factor_all 0.0350 _refine_ls_wR_factor_obs 0.0349 _refine_ls_goodness_of_fit_all 1.183 _refine_ls_goodness_of_fit_obs 1.190 _refine_ls_restrained_S_all 1.183 _refine_ls_restrained_S_obs 1.190 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sm Sm 0.0000 0.0000 0.33386(2) 0.0035(2) Uani 1 d S . Ti Ti 0.0000 0.0000 0.07797(6) 0.0036(3) Uani 1 d S . S S 0.0000 0.0000 0.20374(8) 0.0048(4) Uani 1 d S . O1 O 0.0000 0.5000 0.0976(2) 0.0047(7) Uani 1 d S . O2 O 0.0000 0.0000 0.0000 0.012(2) Uani 1 d S . 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 Sm 0.0031(3) 0.0031(3) 0.0043(3) 0.000 0.000 0.000 Ti 0.0035(4) 0.0035(4) 0.0037(8) 0.000 0.000 0.000 S 0.0041(5) 0.0041(5) 0.0064(10) 0.000 0.000 0.000 O1 0.0061(14) 0.0032(14) 0.005(2) 0.000 0.000 0.000 O2 0.017(3) 0.017(3) 0.003(4) 0.000 0.000 0.000 _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 Sm O1 2.474(3) 27_455 ? Sm O1 2.474(3) 25 ? Sm O1 2.474(3) 27_445 ? Sm O1 2.474(3) 25_455 ? Sm S 2.8343(9) 25_445 ? Sm S 2.8343(9) 25 ? Sm S 2.8343(9) 25_455 ? Sm S 2.8343(9) 25_545 ? Sm S 2.986(2) . ? Sm Ti 3.3741(11) 25 ? Sm Ti 3.3741(11) 25_445 ? Sm Ti 3.3741(11) 25_455 ? Ti O2 1.7895(15) . ? Ti O1 1.9612(11) . ? Ti O1 1.9612(11) 3_655 ? Ti O1 1.9612(11) 3 ? Ti O1 1.9612(11) 1_545 ? Ti S 2.887(2) . ? Ti Sm 3.3741(11) 25 ? Ti Sm 3.3741(11) 25_455 ? Ti Sm 3.3741(11) 25_545 ? Ti Sm 3.3741(11) 25_445 ? S Sm 2.8343(9) 25_445 ? S Sm 2.8343(9) 25 ? S Sm 2.8343(9) 25_455 ? S Sm 2.8343(9) 25_545 ? O1 Ti 1.9612(11) 1_565 ? O1 Sm 2.474(3) 25 ? O1 Sm 2.474(3) 25_455 ? O2 Ti 1.7895(15) 17 ? 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 Sm O1 66.12(8) 27_455 25 ? O1 Sm O1 100.98(15) 27_455 27_445 ? O1 Sm O1 66.12(8) 25 27_445 ? O1 Sm O1 66.12(8) 27_455 25_455 ? O1 Sm O1 100.98(15) 25 25_455 ? O1 Sm O1 66.12(8) 27_445 25_455 ? O1 Sm S 135.51(3) 27_455 25_445 ? O1 Sm S 135.51(3) 25 25_445 ? O1 Sm S 70.98(5) 27_445 25_445 ? O1 Sm S 70.98(5) 25_455 25_445 ? O1 Sm S 70.98(5) 27_455 25 ? O1 Sm S 70.98(5) 25 25 ? O1 Sm S 135.51(3) 27_445 25 ? O1 Sm S 135.51(3) 25_455 25 ? S Sm S 144.55(7) 25_445 25 ? O1 Sm S 70.98(5) 27_455 25_455 ? O1 Sm S 135.51(3) 25 25_455 ? O1 Sm S 135.51(3) 27_445 25_455 ? O1 Sm S 70.98(5) 25_455 25_455 ? S Sm S 84.68(2) 25_445 25_455 ? S Sm S 84.68(2) 25 25_455 ? O1 Sm S 135.51(3) 27_455 25_545 ? O1 Sm S 70.98(5) 25 25_545 ? O1 Sm S 70.98(5) 27_445 25_545 ? O1 Sm S 135.51(3) 25_455 25_545 ? S Sm S 84.68(2) 25_445 25_545 ? S Sm S 84.68(2) 25 25_545 ? S Sm S 144.55(7) 25_455 25_545 ? O1 Sm S 129.51(7) 27_455 . ? O1 Sm S 129.51(7) 25 . ? O1 Sm S 129.51(7) 27_445 . ? O1 Sm S 129.51(7) 25_455 . ? S Sm S 72.27(4) 25_445 . ? S Sm S 72.27(4) 25 . ? S Sm S 72.27(4) 25_455 . ? S Sm S 72.27(4) 25_545 . ? O1 Sm Ti 35.103(15) 27_455 25 ? O1 Sm Ti 35.103(15) 25 25 ? O1 Sm Ti 93.15(6) 27_445 25 ? O1 Sm Ti 93.15(6) 25_455 25 ? S Sm Ti 160.87(5) 25_445 25 ? S Sm Ti 54.58(4) 25 25 ? S Sm Ti 100.52(2) 25_455 25 ? S Sm Ti 100.52(2) 25_545 25 ? S Sm Ti 126.86(2) . 25 ? O1 Sm Ti 93.15(6) 27_455 25_445 ? O1 Sm Ti 93.15(6) 25 25_445 ? O1 Sm Ti 35.103(15) 27_445 25_445 ? O1 Sm Ti 35.103(15) 25_455 25_445 ? S Sm Ti 54.58(4) 25_445 25_445 ? S Sm Ti 160.87(5) 25 25_445 ? S Sm Ti 100.52(2) 25_455 25_445 ? S Sm Ti 100.52(2) 25_545 25_445 ? S Sm Ti 126.86(2) . 25_445 ? Ti Sm Ti 106.29(4) 25 25_445 ? O1 Sm Ti 35.103(15) 27_455 25_455 ? O1 Sm Ti 93.15(6) 25 25_455 ? O1 Sm Ti 93.15(6) 27_445 25_455 ? O1 Sm Ti 35.103(15) 25_455 25_455 ? S Sm Ti 100.52(2) 25_445 25_455 ? S Sm Ti 100.52(2) 25 25_455 ? S Sm Ti 54.58(4) 25_455 25_455 ? S Sm Ti 160.87(5) 25_545 25_455 ? S Sm Ti 126.86(2) . 25_455 ? Ti Sm Ti 68.91(2) 25 25_455 ? Ti Sm Ti 68.91(2) 25_445 25_455 ? O2 Ti O1 103.25(13) . . ? O2 Ti O1 103.25(13) . 3_655 ? O1 Ti O1 86.99(6) . 3_655 ? O2 Ti O1 103.25(13) . 3 ? O1 Ti O1 86.99(6) . 3 ? O1 Ti O1 153.5(3) 3_655 3 ? O2 Ti O1 103.25(13) . 1_545 ? O1 Ti O1 153.5(3) . 1_545 ? O1 Ti O1 86.99(6) 3_655 1_545 ? O1 Ti O1 86.99(6) 3 1_545 ? O2 Ti S 180.0 . . ? O1 Ti S 76.75(13) . . ? O1 Ti S 76.75(13) 3_655 . ? O1 Ti S 76.75(13) 3 . ? O1 Ti S 76.75(13) 1_545 . ? O2 Ti Sm 126.86(2) . 25 ? O1 Ti Sm 46.51(8) . 25 ? O1 Ti Sm 46.51(8) 3_655 25 ? O1 Ti Sm 114.41(10) 3 25 ? O1 Ti Sm 114.41(10) 1_545 25 ? S Ti Sm 53.14(2) . 25 ? O2 Ti Sm 126.86(2) . 25_455 ? O1 Ti Sm 46.51(8) . 25_455 ? O1 Ti Sm 114.41(10) 3_655 25_455 ? O1 Ti Sm 46.51(8) 3 25_455 ? O1 Ti Sm 114.41(10) 1_545 25_455 ? S Ti Sm 53.14(2) . 25_455 ? Sm Ti Sm 68.91(2) 25 25_455 ? O2 Ti Sm 126.86(2) . 25_545 ? O1 Ti Sm 114.41(10) . 25_545 ? O1 Ti Sm 46.51(8) 3_655 25_545 ? O1 Ti Sm 114.41(10) 3 25_545 ? O1 Ti Sm 46.51(8) 1_545 25_545 ? S Ti Sm 53.14(2) . 25_545 ? Sm Ti Sm 68.91(2) 25 25_545 ? Sm Ti Sm 106.29(4) 25_455 25_545 ? O2 Ti Sm 126.86(2) . 25_445 ? O1 Ti Sm 114.41(10) . 25_445 ? O1 Ti Sm 114.41(10) 3_655 25_445 ? O1 Ti Sm 46.51(8) 3 25_445 ? O1 Ti Sm 46.51(8) 1_545 25_445 ? S Ti Sm 53.14(2) . 25_445 ? Sm Ti Sm 106.29(4) 25 25_445 ? Sm Ti Sm 68.91(2) 25_455 25_445 ? Sm Ti Sm 68.91(2) 25_545 25_445 ? Sm S Sm 144.55(7) 25_445 25 ? Sm S Sm 84.68(2) 25_445 25_455 ? Sm S Sm 84.68(2) 25 25_455 ? Sm S Sm 84.68(2) 25_445 25_545 ? Sm S Sm 84.68(2) 25 25_545 ? Sm S Sm 144.55(7) 25_455 25_545 ? Sm S Ti 72.27(4) 25_445 . ? Sm S Ti 72.27(4) 25 . ? Sm S Ti 72.27(4) 25_455 . ? Sm S Ti 72.27(4) 25_545 . ? Sm S Sm 107.73(4) 25_445 . ? Sm S Sm 107.73(4) 25 . ? Sm S Sm 107.73(4) 25_455 . ? Sm S Sm 107.73(4) 25_545 . ? Ti S Sm 180.0 . . ? Ti O1 Ti 153.5(3) . 1_565 ? Ti O1 Sm 98.39(7) . 25 ? Ti O1 Sm 98.39(7) 1_565 25 ? Ti O1 Sm 98.39(7) . 25_455 ? Ti O1 Sm 98.39(7) 1_565 25_455 ? Sm O1 Sm 100.98(15) 25 25_455 ? Ti O2 Ti 180.0 . 17 ? _refine_diff_density_max 0.761 _refine_diff_density_min -1.492 _refine_diff_density_rms 0.187 data_okay2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Nd2 O5 S2 Ti2' _chemical_formula_weight 528.40 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 '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' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 3.8490(10) _cell_length_b 3.8490(10) _cell_length_c 23.064(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 341.69(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.136 _exptl_crystal_density_method ? _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 17.763 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1728 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0146 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 24.68 _reflns_number_total 124 _reflns_number_observed 124 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+0.8271P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0180(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 124 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0168 _refine_ls_R_factor_obs 0.0168 _refine_ls_wR_factor_all 0.0415 _refine_ls_wR_factor_obs 0.0415 _refine_ls_goodness_of_fit_all 1.235 _refine_ls_goodness_of_fit_obs 1.235 _refine_ls_restrained_S_all 1.235 _refine_ls_restrained_S_obs 1.235 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nd Nd 0.0000 0.0000 0.33419(2) 0.0049(4) Uani 1 d S . Ti Ti 0.0000 0.0000 0.07759(8) 0.0059(5) Uani 1 d S . S S 0.0000 0.0000 0.20314(10) 0.0074(6) Uani 1 d S . O1 O 0.0000 0.5000 0.0969(2) 0.0074(10) Uani 1 d S . O2 O 0.0000 0.0000 0.0000 0.023(3) Uani 1 d S . 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 Nd 0.0049(4) 0.0049(4) 0.0050(5) 0.000 0.000 0.000 Ti 0.0069(6) 0.0069(6) 0.0039(9) 0.000 0.000 0.000 S 0.0076(8) 0.0076(8) 0.0072(12) 0.000 0.000 0.000 O1 0.010(2) 0.005(2) 0.007(2) 0.000 0.000 0.000 O2 0.027(5) 0.027(5) 0.015(6) 0.000 0.000 0.000 _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 Nd O1 2.496(3) 27_455 ? Nd O1 2.496(3) 25 ? Nd O1 2.496(3) 27_445 ? Nd O1 2.496(3) 25_455 ? Nd S 2.8546(10) 25_445 ? Nd S 2.8546(10) 25 ? Nd S 2.8546(10) 25_455 ? Nd S 2.8546(10) 25_545 ? Nd S 3.022(2) . ? Nd Ti 3.3981(12) 25 ? Nd Ti 3.3981(12) 25_545 ? Nd Ti 3.3981(12) 25_455 ? Ti O2 1.790(2) . ? Ti O1 1.9755(13) . ? Ti O1 1.9755(13) 3_655 ? Ti O1 1.9755(13) 3 ? Ti O1 1.9755(13) 1_545 ? Ti S 2.896(3) . ? Ti Nd 3.3981(12) 25 ? Ti Nd 3.3981(12) 25_455 ? Ti Nd 3.3981(12) 25_545 ? Ti Nd 3.3981(12) 25_445 ? S Nd 2.8546(10) 25_445 ? S Nd 2.8546(10) 25 ? S Nd 2.8546(10) 25_455 ? S Nd 2.8546(10) 25_545 ? O1 Ti 1.9755(13) 1_565 ? O1 Nd 2.496(3) 25 ? O1 Nd 2.496(3) 25_455 ? O2 Ti 1.790(2) 17 ? 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 Nd O1 66.09(10) 27_455 25 ? O1 Nd O1 100.9(2) 27_455 27_445 ? O1 Nd O1 66.09(10) 25 27_445 ? O1 Nd O1 66.09(10) 27_455 25_455 ? O1 Nd O1 100.9(2) 25 25_455 ? O1 Nd O1 66.09(10) 27_445 25_455 ? O1 Nd S 135.39(4) 27_455 25_445 ? O1 Nd S 135.39(4) 25 25_445 ? O1 Nd S 70.86(7) 27_445 25_445 ? O1 Nd S 70.86(7) 25_455 25_445 ? O1 Nd S 70.86(7) 27_455 25 ? O1 Nd S 70.86(7) 25 25 ? O1 Nd S 135.39(4) 27_445 25 ? O1 Nd S 135.39(4) 25_455 25 ? S Nd S 144.88(9) 25_445 25 ? O1 Nd S 70.86(7) 27_455 25_455 ? O1 Nd S 135.39(4) 25 25_455 ? O1 Nd S 135.39(4) 27_445 25_455 ? O1 Nd S 70.86(7) 25_455 25_455 ? S Nd S 84.78(3) 25_445 25_455 ? S Nd S 84.78(3) 25 25_455 ? O1 Nd S 135.39(4) 27_455 25_545 ? O1 Nd S 70.86(7) 25 25_545 ? O1 Nd S 70.86(7) 27_445 25_545 ? O1 Nd S 135.39(4) 25_455 25_545 ? S Nd S 84.78(3) 25_445 25_545 ? S Nd S 84.78(3) 25 25_545 ? S Nd S 144.88(9) 25_455 25_545 ? O1 Nd S 129.54(9) 27_455 . ? O1 Nd S 129.54(9) 25 . ? O1 Nd S 129.54(9) 27_445 . ? O1 Nd S 129.54(9) 25_455 . ? S Nd S 72.44(4) 25_445 . ? S Nd S 72.44(4) 25 . ? S Nd S 72.44(4) 25_455 . ? S Nd S 72.44(4) 25_545 . ? O1 Nd Ti 35.12(2) 27_455 25 ? O1 Nd Ti 35.12(2) 25 25 ? O1 Nd Ti 93.18(8) 27_445 25 ? O1 Nd Ti 93.18(8) 25_455 25 ? S Nd Ti 160.78(5) 25_445 25 ? S Nd Ti 54.34(5) 25 25 ? S Nd Ti 100.41(3) 25_455 25 ? S Nd Ti 100.41(3) 25_545 25 ? S Nd Ti 126.78(2) . 25 ? O1 Nd Ti 93.18(8) 27_455 25_545 ? O1 Nd Ti 35.12(2) 25 25_545 ? O1 Nd Ti 35.12(2) 27_445 25_545 ? O1 Nd Ti 93.18(8) 25_455 25_545 ? S Nd Ti 100.41(3) 25_445 25_545 ? S Nd Ti 100.41(3) 25 25_545 ? S Nd Ti 160.78(5) 25_455 25_545 ? S Nd Ti 54.34(5) 25_545 25_545 ? S Nd Ti 126.78(2) . 25_545 ? Ti Nd Ti 68.99(3) 25 25_545 ? O1 Nd Ti 35.12(2) 27_455 25_455 ? O1 Nd Ti 93.18(8) 25 25_455 ? O1 Nd Ti 93.18(8) 27_445 25_455 ? O1 Nd Ti 35.12(2) 25_455 25_455 ? S Nd Ti 100.41(3) 25_445 25_455 ? S Nd Ti 100.41(3) 25 25_455 ? S Nd Ti 54.34(5) 25_455 25_455 ? S Nd Ti 160.78(5) 25_545 25_455 ? S Nd Ti 126.78(2) . 25_455 ? Ti Nd Ti 68.99(3) 25 25_455 ? Ti Nd Ti 106.44(5) 25_545 25_455 ? O2 Ti O1 103.04(15) . . ? O2 Ti O1 103.04(15) . 3_655 ? O1 Ti O1 87.08(7) . 3_655 ? O2 Ti O1 103.04(15) . 3 ? O1 Ti O1 87.08(7) . 3 ? O1 Ti O1 153.9(3) 3_655 3 ? O2 Ti O1 103.04(15) . 1_545 ? O1 Ti O1 153.9(3) . 1_545 ? O1 Ti O1 87.08(7) 3_655 1_545 ? O1 Ti O1 87.08(7) 3 1_545 ? O2 Ti S 180.0 . . ? O1 Ti S 76.96(15) . . ? O1 Ti S 76.96(15) 3_655 . ? O1 Ti S 76.96(15) 3 . ? O1 Ti S 76.96(15) 1_545 . ? O2 Ti Nd 126.78(2) . 25 ? O1 Ti Nd 46.62(9) . 25 ? O1 Ti Nd 46.62(9) 3_655 25 ? O1 Ti Nd 114.62(12) 3 25 ? O1 Ti Nd 114.62(12) 1_545 25 ? S Ti Nd 53.22(2) . 25 ? O2 Ti Nd 126.78(2) . 25_455 ? O1 Ti Nd 46.62(9) . 25_455 ? O1 Ti Nd 114.62(12) 3_655 25_455 ? O1 Ti Nd 46.62(9) 3 25_455 ? O1 Ti Nd 114.62(12) 1_545 25_455 ? S Ti Nd 53.22(2) . 25_455 ? Nd Ti Nd 68.99(3) 25 25_455 ? O2 Ti Nd 126.78(2) . 25_545 ? O1 Ti Nd 114.62(12) . 25_545 ? O1 Ti Nd 46.62(9) 3_655 25_545 ? O1 Ti Nd 114.62(12) 3 25_545 ? O1 Ti Nd 46.62(9) 1_545 25_545 ? S Ti Nd 53.22(2) . 25_545 ? Nd Ti Nd 68.99(3) 25 25_545 ? Nd Ti Nd 106.44(5) 25_455 25_545 ? O2 Ti Nd 126.78(2) . 25_445 ? O1 Ti Nd 114.62(12) . 25_445 ? O1 Ti Nd 114.62(12) 3_655 25_445 ? O1 Ti Nd 46.62(9) 3 25_445 ? O1 Ti Nd 46.62(9) 1_545 25_445 ? S Ti Nd 53.22(2) . 25_445 ? Nd Ti Nd 106.44(5) 25 25_445 ? Nd Ti Nd 68.99(3) 25_455 25_445 ? Nd Ti Nd 68.99(3) 25_545 25_445 ? Nd S Nd 144.88(9) 25_445 25 ? Nd S Nd 84.78(3) 25_445 25_455 ? Nd S Nd 84.78(3) 25 25_455 ? Nd S Nd 84.78(3) 25_445 25_545 ? Nd S Nd 84.78(3) 25 25_545 ? Nd S Nd 144.88(9) 25_455 25_545 ? Nd S Ti 72.44(4) 25_445 . ? Nd S Ti 72.44(4) 25 . ? Nd S Ti 72.44(4) 25_455 . ? Nd S Ti 72.44(4) 25_545 . ? Nd S Nd 107.56(4) 25_445 . ? Nd S Nd 107.56(4) 25 . ? Nd S Nd 107.56(4) 25_455 . ? Nd S Nd 107.56(4) 25_545 . ? Ti S Nd 180.0 . . ? Ti O1 Ti 153.9(3) . 1_565 ? Ti O1 Nd 98.26(8) . 25 ? Ti O1 Nd 98.26(8) 1_565 25 ? Ti O1 Nd 98.26(8) . 25_455 ? Ti O1 Nd 98.26(8) 1_565 25_455 ? Nd O1 Nd 100.9(2) 25 25_455 ? Ti O2 Ti 180.0 17 . ? _refine_diff_density_max 1.020 _refine_diff_density_min -1.125 _refine_diff_density_rms 0.195 data_okay3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'O5 Pr2 S2 Ti2' _chemical_formula_weight 521.74 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 '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' 'Pr' 'Pr' -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 3.8710(10) _cell_length_b 3.8710(10) _cell_length_c 23.036(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 345.19(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 35 _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.020 _exptl_crystal_density_method ? _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 16.656 _exptl_absorpt_correction_type 'Semi-empirical from psi-scans' _exptl_absorpt_correction_T_min 0.52 _exptl_absorpt_correction_T_max 0.99 _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 'P21 four-circle diffractometer' _diffrn_measurement_method theta-2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 764 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 5.34 _diffrn_reflns_theta_max 35.08 _reflns_number_total 243 _reflns_number_observed 232 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'P21 data collections programs' _computing_cell_refinement 'P21 data collection programs' _computing_data_reduction 'SHELXTL (Siemens, 1986)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Diamond' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+4.5035P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 243 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_obs 0.0291 _refine_ls_wR_factor_all 0.0696 _refine_ls_wR_factor_obs 0.0686 _refine_ls_goodness_of_fit_all 1.195 _refine_ls_goodness_of_fit_obs 1.208 _refine_ls_restrained_S_all 1.195 _refine_ls_restrained_S_obs 1.208 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pr Pr 0.0000 0.0000 0.33434(3) 0.0074(2) Uani 1 d S . Ti Ti 0.0000 0.0000 0.07796(9) 0.0087(3) Uani 1 d S . S S 0.0000 0.0000 0.20301(12) 0.0096(5) Uani 1 d S . O1 O 0.0000 0.5000 0.0967(2) 0.0098(9) Uani 1 d S . O2 O 0.0000 0.0000 0.0000 0.017(3) Uani 1 d S . 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 Pr 0.0065(2) 0.0065(2) 0.0091(3) 0.000 0.000 0.000 Ti 0.0093(5) 0.0093(5) 0.0076(8) 0.000 0.000 0.000 S 0.0083(6) 0.0083(6) 0.0122(11) 0.000 0.000 0.000 O1 0.011(2) 0.009(2) 0.010(2) 0.000 0.000 0.000 O2 0.022(4) 0.022(4) 0.008(5) 0.000 0.000 0.000 _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 Pr O1 2.505(4) 27_455 ? Pr O1 2.505(4) 25 ? Pr O1 2.505(4) 27_445 ? Pr O1 2.505(4) 25_455 ? Pr S 2.8692(11) 25_445 ? Pr S 2.8692(11) 25 ? Pr S 2.8692(11) 25_455 ? Pr S 2.8692(11) 25_545 ? Pr S 3.025(3) . ? Pr Ti 3.4021(14) 25 ? Pr Ti 3.4021(14) 25_545 ? Pr Ti 3.4021(14) 25_455 ? Ti O2 1.796(2) . ? Ti O1 1.9828(14) 3_655 ? Ti O1 1.9828(14) . ? Ti O1 1.9828(14) 3 ? Ti O1 1.9828(14) 1_545 ? Ti S 2.881(3) . ? Ti Pr 3.4021(14) 25 ? Ti Pr 3.4021(14) 25_455 ? Ti Pr 3.4021(14) 25_545 ? Ti Pr 3.4021(14) 25_445 ? S Pr 2.8692(11) 25_445 ? S Pr 2.8692(11) 25 ? S Pr 2.8692(11) 25_455 ? S Pr 2.8692(11) 25_545 ? O1 Ti 1.9828(14) 1_565 ? O1 Pr 2.505(4) 25 ? O1 Pr 2.505(4) 25_455 ? O2 Ti 1.796(2) 17 ? 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 Pr O1 66.25(11) 27_455 25 ? O1 Pr O1 101.2(2) 27_455 27_445 ? O1 Pr O1 66.25(11) 25 27_445 ? O1 Pr O1 66.25(11) 27_455 25_455 ? O1 Pr O1 101.2(2) 25 25_455 ? O1 Pr O1 66.25(11) 27_445 25_455 ? O1 Pr S 135.37(5) 27_455 25_445 ? O1 Pr S 135.37(5) 25 25_445 ? O1 Pr S 70.67(8) 27_445 25_445 ? O1 Pr S 70.67(8) 25_455 25_445 ? O1 Pr S 70.67(8) 27_455 25 ? O1 Pr S 70.67(8) 25 25 ? O1 Pr S 135.37(5) 27_445 25 ? O1 Pr S 135.37(5) 25_455 25 ? S Pr S 145.10(11) 25_445 25 ? O1 Pr S 70.67(8) 27_455 25_455 ? O1 Pr S 135.37(5) 25 25_455 ? O1 Pr S 135.37(5) 27_445 25_455 ? O1 Pr S 70.67(8) 25_455 25_455 ? S Pr S 84.84(3) 25_445 25_455 ? S Pr S 84.84(3) 25 25_455 ? O1 Pr S 135.37(5) 27_455 25_545 ? O1 Pr S 70.67(8) 25 25_545 ? O1 Pr S 70.67(8) 27_445 25_545 ? O1 Pr S 135.37(5) 25_455 25_545 ? S Pr S 84.84(3) 25_445 25_545 ? S Pr S 84.84(3) 25 25_545 ? S Pr S 145.10(11) 25_455 25_545 ? O1 Pr S 129.40(10) 27_455 . ? O1 Pr S 129.40(10) 25 . ? O1 Pr S 129.40(10) 27_445 . ? O1 Pr S 129.40(10) 25_455 . ? S Pr S 72.55(6) 25_445 . ? S Pr S 72.55(6) 25 . ? S Pr S 72.55(6) 25_455 . ? S Pr S 72.55(6) 25_545 . ? O1 Pr Ti 35.26(2) 27_455 25 ? O1 Pr Ti 35.26(2) 25 25 ? O1 Pr Ti 93.60(9) 27_445 25 ? O1 Pr Ti 93.60(9) 25_455 25 ? S Pr Ti 161.02(7) 25_445 25 ? S Pr Ti 53.88(6) 25 25 ? S Pr Ti 100.26(3) 25_455 25 ? S Pr Ti 100.26(3) 25_545 25 ? S Pr Ti 126.43(3) . 25 ? O1 Pr Ti 93.60(9) 27_455 25_545 ? O1 Pr Ti 35.26(2) 25 25_545 ? O1 Pr Ti 35.26(2) 27_445 25_545 ? O1 Pr Ti 93.60(9) 25_455 25_545 ? S Pr Ti 100.26(3) 25_445 25_545 ? S Pr Ti 100.26(3) 25 25_545 ? S Pr Ti 161.02(7) 25_455 25_545 ? S Pr Ti 53.88(6) 25_545 25_545 ? S Pr Ti 126.43(3) . 25_545 ? Ti Pr Ti 69.35(3) 25 25_545 ? O1 Pr Ti 35.26(2) 27_455 25_455 ? O1 Pr Ti 93.60(9) 25 25_455 ? O1 Pr Ti 93.60(9) 27_445 25_455 ? O1 Pr Ti 35.26(2) 25_455 25_455 ? S Pr Ti 100.26(3) 25_445 25_455 ? S Pr Ti 100.26(3) 25 25_455 ? S Pr Ti 53.88(6) 25_455 25_455 ? S Pr Ti 161.02(7) 25_545 25_455 ? S Pr Ti 126.43(3) . 25_455 ? Ti Pr Ti 69.35(3) 25 25_455 ? Ti Pr Ti 107.14(6) 25_545 25_455 ? O2 Ti O1 102.5(2) . 3_655 ? O2 Ti O1 102.5(2) . . ? O1 Ti O1 87.30(7) 3_655 . ? O2 Ti O1 102.5(2) . 3 ? O1 Ti O1 154.9(3) 3_655 3 ? O1 Ti O1 87.30(7) . 3 ? O2 Ti O1 102.5(2) . 1_545 ? O1 Ti O1 87.30(7) 3_655 1_545 ? O1 Ti O1 154.9(3) . 1_545 ? O1 Ti O1 87.30(7) 3 1_545 ? O2 Ti S 180.0 . . ? O1 Ti S 77.5(2) 3_655 . ? O1 Ti S 77.5(2) . . ? O1 Ti S 77.5(2) 3 . ? O1 Ti S 77.5(2) 1_545 . ? O2 Ti Pr 126.43(3) . 25 ? O1 Ti Pr 46.82(10) 3_655 25 ? O1 Ti Pr 46.82(10) . 25 ? O1 Ti Pr 115.24(13) 3 25 ? O1 Ti Pr 115.24(13) 1_545 25 ? S Ti Pr 53.57(3) . 25 ? O2 Ti Pr 126.43(3) . 25_455 ? O1 Ti Pr 115.24(13) 3_655 25_455 ? O1 Ti Pr 46.82(10) . 25_455 ? O1 Ti Pr 46.82(10) 3 25_455 ? O1 Ti Pr 115.24(13) 1_545 25_455 ? S Ti Pr 53.57(3) . 25_455 ? Pr Ti Pr 69.35(3) 25 25_455 ? O2 Ti Pr 126.43(3) . 25_545 ? O1 Ti Pr 46.82(10) 3_655 25_545 ? O1 Ti Pr 115.24(13) . 25_545 ? O1 Ti Pr 115.24(13) 3 25_545 ? O1 Ti Pr 46.82(10) 1_545 25_545 ? S Ti Pr 53.57(3) . 25_545 ? Pr Ti Pr 69.35(3) 25 25_545 ? Pr Ti Pr 107.14(6) 25_455 25_545 ? O2 Ti Pr 126.43(3) . 25_445 ? O1 Ti Pr 115.24(13) 3_655 25_445 ? O1 Ti Pr 115.24(13) . 25_445 ? O1 Ti Pr 46.82(10) 3 25_445 ? O1 Ti Pr 46.82(10) 1_545 25_445 ? S Ti Pr 53.57(3) . 25_445 ? Pr Ti Pr 107.14(6) 25 25_445 ? Pr Ti Pr 69.35(3) 25_455 25_445 ? Pr Ti Pr 69.35(3) 25_545 25_445 ? Pr S Pr 145.10(11) 25_445 25 ? Pr S Pr 84.84(3) 25_445 25_455 ? Pr S Pr 84.84(3) 25 25_455 ? Pr S Pr 84.84(3) 25_445 25_545 ? Pr S Pr 84.84(3) 25 25_545 ? Pr S Pr 145.10(11) 25_455 25_545 ? Pr S Ti 72.55(6) 25_445 . ? Pr S Ti 72.55(6) 25 . ? Pr S Ti 72.55(6) 25_455 . ? Pr S Ti 72.55(6) 25_545 . ? Pr S Pr 107.45(6) 25_445 . ? Pr S Pr 107.45(6) 25 . ? Pr S Pr 107.45(6) 25_455 . ? Pr S Pr 107.45(6) 25_545 . ? Ti S Pr 180.0 . . ? Ti O1 Ti 154.9(3) . 1_565 ? Ti O1 Pr 97.92(9) . 25 ? Ti O1 Pr 97.92(9) 1_565 25 ? Ti O1 Pr 97.92(9) . 25_455 ? Ti O1 Pr 97.92(9) 1_565 25_455 ? Pr O1 Pr 101.2(2) 25 25_455 ? Ti O2 Ti 180.0 . 17 ? _refine_diff_density_max 8.268 _refine_diff_density_min -1.753 _refine_diff_density_rms 0.382