data_shelxl _audit_creation_method 'SHELXL-2018/1' _chemical_name_systematic ; ? ; _chemical_name_common 'thorasphite' _chemical_formula_moiety 'As1.50 O18 P1.50 Th2' _chemical_formula_sum 'As1.50 O18 P1.50 Th2' _chemical_formula_weight 910.91 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Th' 'Th' -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pbcn' _symmetry_space_group_name_Hall '-P 2ac 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.673(3) _cell_length_b 9.925(2) _cell_length_c 10.222(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1387.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9250 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.46 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.002 _exptl_crystal_size_min 0.002 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 26.154 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_type 'ADSC Quantum 210r' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 21723 _diffrn_reflns_av_R_equivalents 0.2265 _diffrn_reflns_av_sigmaI/netI 0.0985 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 30.05 _reflns_number_total 1970 _reflns_number_gt 1432 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1437P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1970 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2196 _refine_ls_wR_factor_gt 0.1934 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Th1 Th 0.11772(4) 0.14113(6) 0.47734(5) 0.0316(3) Uani 0.987(17) 1 d P . . P P 0.0000 0.1154(5) 0.7500 0.0300(15) Uani 1 2 d SP . . As As 0.14272(14) 0.7829(2) 0.61414(18) 0.0269(7) Uani 0.676(13) 1 d P . . O1 O 0.0893(9) 0.2003(14) 0.7059(11) 0.043(3) Uani 1 1 d . . . O2 O 0.0227(8) 0.0230(12) 0.8697(10) 0.036(2) Uani 1 1 d . . . O3 O 0.0361(8) 0.7513(14) 0.5563(11) 0.042(3) Uani 1 1 d . . . O4 O 0.2227(8) 0.6905(15) 0.5400(10) 0.040(3) Uani 1 1 d . . . O5 O 0.1457(9) 0.7566(15) 0.7733(11) 0.049(3) Uani 1 1 d . . . O6 O 0.1751(7) 0.9403(12) 0.5850(11) 0.037(3) Uani 1 1 d . . . O7 O 0.1251(10) 0.401(2) 0.5210(15) 0.054(4) Uani 1 1 d . . . O8 O 0.2361(9) -0.0013(15) 0.3268(11) 0.048(3) Uani 1 1 d . . . O9 O 0.0626(9) 0.5654(14) 0.3426(13) 0.054(4) 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 Th1 0.0273(4) 0.0455(5) 0.0221(4) 0.00099(19) -0.00140(16) -0.0021(2) P 0.029(2) 0.043(3) 0.0178(19) 0.000 -0.0016(15) 0.000 As 0.0238(10) 0.0383(13) 0.0187(9) -0.0023(7) 0.0016(7) 0.0010(8) O2 0.035(5) 0.043(6) 0.030(5) 0.004(4) 0.003(4) 0.007(4) O1 0.043(6) 0.060(8) 0.025(5) -0.004(5) 0.009(4) -0.007(6) O3 0.031(5) 0.053(7) 0.043(6) 0.000(6) 0.002(5) 0.010(5) O4 0.031(6) 0.061(8) 0.029(5) -0.014(5) 0.005(4) -0.013(5) O5 0.048(6) 0.071(9) 0.027(5) -0.007(6) 0.011(5) 0.003(6) O6 0.034(5) 0.045(7) 0.031(5) 0.007(5) -0.001(4) -0.007(5) O7 0.046(9) 0.065(10) 0.052(10) 0.008(7) 0.007(5) 0.003(7) O8 0.047(6) 0.061(8) 0.035(6) -0.001(6) -0.006(5) 0.011(6) O9 0.057(7) 0.056(8) 0.048(7) 0.031(6) 0.024(6) 0.025(6) _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 Th1 O4 2.327(11) 8_655 ? Th1 O5 2.351(11) 7_565 ? Th1 O2 2.356(11) 7 ? Th1 O3 2.384(11) 5_566 ? Th1 O6 2.408(12) 1_545 ? Th1 O1 2.440(11) . ? Th1 O7 2.62(2) . ? Th1 O8 2.644(13) . ? Th1 O2 2.740(10) 3_556 ? Th1 P 3.2287(8) . ? P O1 1.550(12) . ? P O1 1.550(12) 3_556 ? P O2 1.560(11) . ? P O2 1.560(11) 3_556 ? P Th1 3.2287(8) 3_556 ? As O3 1.604(11) . ? As O4 1.615(12) . ? As O5 1.648(11) . ? As O6 1.650(12) . ? O2 Th1 2.356(11) 7_556 ? O2 Th1 2.740(10) 3_556 ? O3 Th1 2.384(11) 5_566 ? O4 Th1 2.327(11) 8_665 ? O5 Th1 2.351(11) 7_566 ? O6 Th1 2.408(12) 1_565 ? 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 O4 Th1 O5 90.0(4) 8_655 7_565 ? O4 Th1 O2 142.3(4) 8_655 7 ? O5 Th1 O2 88.5(4) 7_565 7 ? O4 Th1 O3 140.6(5) 8_655 5_566 ? O5 Th1 O3 79.8(4) 7_565 5_566 ? O2 Th1 O3 75.9(4) 7 5_566 ? O4 Th1 O6 75.1(4) 8_655 1_545 ? O5 Th1 O6 135.2(4) 7_565 1_545 ? O2 Th1 O6 79.7(4) 7 1_545 ? O3 Th1 O6 136.4(4) 5_566 1_545 ? O4 Th1 O1 80.5(4) 8_655 . ? O5 Th1 O1 140.5(5) 7_565 . ? O2 Th1 O1 121.7(4) 7 . ? O3 Th1 O1 83.7(4) 5_566 . ? O6 Th1 O1 79.2(4) 1_545 . ? O4 Th1 O7 73.1(5) 8_655 . ? O5 Th1 O7 73.7(5) 7_565 . ? O2 Th1 O7 141.4(5) 7 . ? O3 Th1 O7 67.5(5) 5_566 . ? O6 Th1 O7 136.4(4) 1_545 . ? O1 Th1 O7 66.8(5) . . ? O4 Th1 O8 72.5(4) 8_655 . ? O5 Th1 O8 67.3(4) 7_565 . ? O2 Th1 O8 72.3(4) 7 . ? O3 Th1 O8 134.1(4) 5_566 . ? O6 Th1 O8 67.9(4) 1_545 . ? O1 Th1 O8 141.6(4) . . ? O7 Th1 O8 127.0(5) . . ? O4 Th1 O2 126.2(4) 8_655 3_556 ? O5 Th1 O2 143.6(4) 7_565 3_556 ? O2 Th1 O2 65.4(4) 7 3_556 ? O3 Th1 O2 69.9(4) 5_566 3_556 ? O6 Th1 O2 67.2(4) 1_545 3_556 ? O1 Th1 O2 56.3(4) . 3_556 ? O7 Th1 O2 110.6(4) . 3_556 ? O8 Th1 O2 122.2(4) . 3_556 ? O4 Th1 P 104.3(3) 8_655 . ? O5 Th1 P 151.8(3) 7_565 . ? O2 Th1 P 94.2(3) 7 . ? O3 Th1 P 73.7(3) 5_566 . ? O6 Th1 P 72.7(3) 1_545 . ? O1 Th1 P 27.5(3) . . ? O7 Th1 P 87.1(3) . . ? O8 Th1 P 140.0(3) . . ? O2 Th1 P 28.9(2) 3_556 . ? O1 P O1 114.2(11) . 3_556 ? O1 P O2 113.0(6) . . ? O1 P O2 104.4(6) 3_556 . ? O1 P O2 104.4(6) . 3_556 ? O1 P O2 113.0(6) 3_556 3_556 ? O2 P O2 108.0(9) . 3_556 ? O1 P Th1 126.9(5) . 3_556 ? O1 P Th1 46.6(4) 3_556 3_556 ? O2 P Th1 57.9(4) . 3_556 ? O2 P Th1 128.6(4) 3_556 3_556 ? O1 P Th1 46.6(4) . . ? O1 P Th1 126.9(5) 3_556 . ? O2 P Th1 128.6(4) . . ? O2 P Th1 57.9(4) 3_556 . ? Th1 P Th1 170.94(18) 3_556 . ? O3 As O4 109.3(6) . . ? O3 As O5 110.8(6) . . ? O4 As O5 110.9(6) . . ? O3 As O6 111.2(6) . . ? O4 As O6 105.7(6) . . ? O5 As O6 108.7(7) . . ? P O2 Th1 151.9(6) . 7_556 ? P O2 Th1 93.2(5) . 3_556 ? Th1 O2 Th1 114.6(4) 7_556 3_556 ? P O1 Th1 105.9(6) . . ? As O3 Th1 140.1(8) . 5_566 ? As O4 Th1 152.0(7) . 8_665 ? As O5 Th1 143.5(8) . 7_566 ? As O6 Th1 141.1(6) . 1_565 ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 4.631 _refine_diff_density_min -3.570 _refine_diff_density_rms 0.828