#=============================================================================== data_global #=============================================================================== _audit_creation_date 'July 26, 2017' _audit_creation_method 'manual editing of .cif file' _audit_update_record ; ; #=============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Dr. Jakoah Brgoch' _publ_contact_author_address ; Department of Chemistry University of Alberta Edmonton, AB Canada T6G 2G2 ; _publ_contact_author_phone '(713) 743 6233' _publ_contact_author_email jbrgoch@uh.edu _publ_requested_journal 'JACS' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #=============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Frustrated Machine Learning: Structure Prediction and Polymorphism in Titanium Iron Phosphide ; _publ_section_title_footnote . loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Oliynyk, Anton O.' ; ? ; ; Department of Chemistry University of Houston Houston, TX USA 77004 ; 'Brgoch, Jakoah' ; ? ; ; Department of Chemistry University of Houston Houston, TX USA 77004 ; #=============================================================================== # TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgments ; ? ; #=============================================================================== data_TiFeP_(TiNiSi-type) _audit_creation_method SHELXL-97 _chemical_name_systematic 'titanium iron phosphide (1/1/1)' _chemical_name_common 'titanium iron phosphide (1/1/1)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Fe P Ti' _chemical_formula_structural 'Ti Fe P' _chemical_formula_weight 134.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'P' 'P' 0.1023 0.0942 '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 5.9865(9) _cell_length_b 3.5976(6) _cell_length_c 6.8640(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 147.83(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1257 _cell_measurement_theta_min 4.5175 _cell_measurement_theta_max 29.016 _exptl_crystal_description prism _exptl_crystal_colour grey _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 252 _exptl_absorpt_coefficient_mu 15.585 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.61001 _exptl_absorpt_correction_T_max 0.77313 _exptl_absorpt_process_details 'Bruker SHELXTL 6.12 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker D8/SMART APEX II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 1982 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.52 _diffrn_reflns_theta_max 33.11 _reflns_number_total 316 _reflns_number_gt 280 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Bruker SMART 5.054 (Bruker, 1999)' _computing_cell_refinement 'Bruker SAINT 7.06A (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT 7.06A' _computing_structure_solution 'Bruker SHELXTL 6.12' _computing_structure_refinement 'Bruker SHELXTL 6.12' _computing_molecular_graphics 'ATOMS 5.1 (Dowty, 1999)' _computing_publication_material 'Bruker SHELXTL 6.12' _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^)+(0.0481P)^2^+2.8955P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 316 _refine_ls_number_parameters 19 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _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 Fe1 Fe 0.14734(18) 0.2500 0.06088(16) 0.0084(3) Uani 1 2 d S . . Ti2 Ti 0.0253(2) 0.2500 0.67692(19) 0.0070(3) Uani 1 2 d S . . P3 P 0.2703(3) 0.2500 0.3760(3) 0.0074(4) Uani 1 2 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 Fe1 0.0077(5) 0.0080(5) 0.0095(5) 0.000 0.0003(4) 0.000 Ti2 0.0058(6) 0.0074(6) 0.0078(5) 0.000 0.0003(4) 0.000 P3 0.0067(8) 0.0067(8) 0.0089(8) 0.000 -0.0005(6) 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 Fe1 P3 2.2559(14) 2_554 ? Fe1 P3 2.2559(14) 2_564 ? Fe1 P3 2.285(2) . ? Fe1 P3 2.298(2) 6_556 ? Fe1 Fe1 2.6545(16) 5 ? Fe1 Fe1 2.6545(16) 5_565 ? Fe1 Ti2 2.7348(17) 1_554 ? Fe1 Ti2 2.7465(13) 5_566 ? Fe1 Ti2 2.7465(13) 5_556 ? Fe1 Ti2 2.7767(13) 2_564 ? Fe1 Ti2 2.7767(13) 2_554 ? Fe1 Ti2 2.7901(17) 6_656 ? Ti2 P3 2.533(2) . ? Ti2 P3 2.5494(16) 5_556 ? Ti2 P3 2.5494(16) 5_566 ? Ti2 P3 2.5692(17) 2_565 ? Ti2 P3 2.5692(17) 2 ? Ti2 Fe1 2.7348(18) 1_556 ? Ti2 Fe1 2.7466(13) 5_566 ? Ti2 Fe1 2.7466(13) 5_556 ? Ti2 Fe1 2.7767(14) 2_565 ? Ti2 Fe1 2.7767(13) 2 ? Ti2 Fe1 2.7901(17) 6_556 ? Ti2 Ti2 3.037(2) 5_556 ? P3 Fe1 2.2558(14) 2_565 ? P3 Fe1 2.2558(14) 2 ? P3 Fe1 2.298(2) 6_656 ? P3 Ti2 2.5494(16) 5_556 ? P3 Ti2 2.5494(16) 5_566 ? P3 Ti2 2.5692(17) 2_554 ? P3 Ti2 2.5692(17) 2_564 ? 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 P3 Fe1 P3 105.76(9) 2_554 2_564 ? P3 Fe1 P3 117.52(5) 2_554 . ? P3 Fe1 P3 117.52(5) 2_564 . ? P3 Fe1 P3 108.71(6) 2_554 6_556 ? P3 Fe1 P3 108.71(6) 2_564 6_556 ? P3 Fe1 P3 97.93(6) . 6_556 ? P3 Fe1 Fe1 55.10(5) 2_554 5 ? P3 Fe1 Fe1 120.57(8) 2_564 5 ? P3 Fe1 Fe1 120.80(6) . 5 ? P3 Fe1 Fe1 53.61(5) 6_556 5 ? P3 Fe1 Fe1 120.57(8) 2_554 5_565 ? P3 Fe1 Fe1 55.10(5) 2_564 5_565 ? P3 Fe1 Fe1 120.80(6) . 5_565 ? P3 Fe1 Fe1 53.61(5) 6_556 5_565 ? Fe1 Fe1 Fe1 85.32(7) 5 5_565 ? P3 Fe1 Ti2 61.08(5) 2_554 1_554 ? P3 Fe1 Ti2 61.08(5) 2_564 1_554 ? P3 Fe1 Ti2 176.70(7) . 1_554 ? P3 Fe1 Ti2 85.37(7) 6_556 1_554 ? Fe1 Fe1 Ti2 61.26(4) 5 1_554 ? Fe1 Fe1 Ti2 61.26(4) 5_565 1_554 ? P3 Fe1 Ti2 166.68(6) 2_554 5_566 ? P3 Fe1 Ti2 85.91(5) 2_564 5_566 ? P3 Fe1 Ti2 60.06(5) . 5_566 ? P3 Fe1 Ti2 60.45(5) 6_556 5_566 ? Fe1 Fe1 Ti2 113.58(7) 5 5_566 ? Fe1 Fe1 Ti2 60.81(4) 5_565 5_566 ? Ti2 Fe1 Ti2 122.07(4) 1_554 5_566 ? P3 Fe1 Ti2 85.91(5) 2_554 5_556 ? P3 Fe1 Ti2 166.68(6) 2_564 5_556 ? P3 Fe1 Ti2 60.06(5) . 5_556 ? P3 Fe1 Ti2 60.45(5) 6_556 5_556 ? Fe1 Fe1 Ti2 60.81(4) 5 5_556 ? Fe1 Fe1 Ti2 113.58(7) 5_565 5_556 ? Ti2 Fe1 Ti2 122.07(4) 1_554 5_556 ? Ti2 Fe1 Ti2 81.83(5) 5_566 5_556 ? P3 Fe1 Ti2 121.58(7) 2_554 2_564 ? P3 Fe1 Ti2 59.37(6) 2_564 2_564 ? P3 Fe1 Ti2 60.07(4) . 2_564 ? P3 Fe1 Ti2 129.72(5) 6_556 2_564 ? Fe1 Fe1 Ti2 176.68(7) 5 2_564 ? Fe1 Fe1 Ti2 96.91(3) 5_565 2_564 ? Ti2 Fe1 Ti2 117.70(5) 1_554 2_564 ? Ti2 Fe1 Ti2 69.72(2) 5_566 2_564 ? Ti2 Fe1 Ti2 120.13(4) 5_556 2_564 ? P3 Fe1 Ti2 59.37(6) 2_554 2_554 ? P3 Fe1 Ti2 121.58(7) 2_564 2_554 ? P3 Fe1 Ti2 60.07(4) . 2_554 ? P3 Fe1 Ti2 129.72(5) 6_556 2_554 ? Fe1 Fe1 Ti2 96.91(3) 5 2_554 ? Fe1 Fe1 Ti2 176.68(7) 5_565 2_554 ? Ti2 Fe1 Ti2 117.70(5) 1_554 2_554 ? Ti2 Fe1 Ti2 120.13(4) 5_566 2_554 ? Ti2 Fe1 Ti2 69.72(2) 5_556 2_554 ? Ti2 Fe1 Ti2 80.76(5) 2_564 2_554 ? P3 Fe1 Ti2 59.58(5) 2_554 6_656 ? P3 Fe1 Ti2 59.58(5) 2_564 6_656 ? P3 Fe1 Ti2 107.01(7) . 6_656 ? P3 Fe1 Ti2 155.06(7) 6_556 6_656 ? Fe1 Fe1 Ti2 110.78(6) 5 6_656 ? Fe1 Fe1 Ti2 110.78(6) 5_565 6_656 ? Ti2 Fe1 Ti2 69.69(3) 1_554 6_656 ? Ti2 Fe1 Ti2 133.52(3) 5_566 6_656 ? Ti2 Fe1 Ti2 133.52(3) 5_556 6_656 ? Ti2 Fe1 Ti2 66.14(4) 2_564 6_656 ? Ti2 Fe1 Ti2 66.14(4) 2_554 6_656 ? P3 Ti2 P3 106.60(6) . 5_556 ? P3 Ti2 P3 106.60(6) . 5_566 ? P3 Ti2 P3 89.75(7) 5_556 5_566 ? P3 Ti2 P3 99.09(4) . 2_565 ? P3 Ti2 P3 154.21(7) 5_556 2_565 ? P3 Ti2 P3 84.97(4) 5_566 2_565 ? P3 Ti2 P3 99.09(4) . 2 ? P3 Ti2 P3 84.97(4) 5_556 2 ? P3 Ti2 P3 154.21(7) 5_566 2 ? P3 Ti2 P3 88.88(7) 2_565 2 ? P3 Ti2 Fe1 129.14(7) . 1_556 ? P3 Ti2 Fe1 108.83(6) 5_556 1_556 ? P3 Ti2 Fe1 108.83(6) 5_566 1_556 ? P3 Ti2 Fe1 50.22(4) 2_565 1_556 ? P3 Ti2 Fe1 50.22(4) 2 1_556 ? P3 Ti2 Fe1 138.78(3) . 5_566 ? P3 Ti2 Fe1 107.11(6) 5_556 5_566 ? P3 Ti2 Fe1 50.95(5) 5_566 5_566 ? P3 Ti2 Fe1 51.11(5) 2_565 5_566 ? P3 Ti2 Fe1 106.81(6) 2 5_566 ? Fe1 Ti2 Fe1 57.93(4) 1_556 5_566 ? P3 Ti2 Fe1 138.78(3) . 5_556 ? P3 Ti2 Fe1 50.95(5) 5_556 5_556 ? P3 Ti2 Fe1 107.11(6) 5_566 5_556 ? P3 Ti2 Fe1 106.81(6) 2_565 5_556 ? P3 Ti2 Fe1 51.11(5) 2 5_556 ? Fe1 Ti2 Fe1 57.93(4) 1_556 5_556 ? Fe1 Ti2 Fe1 81.83(5) 5_566 5_556 ? P3 Ti2 Fe1 50.03(4) . 2_565 ? P3 Ti2 Fe1 154.97(8) 5_556 2_565 ? P3 Ti2 Fe1 89.54(4) 5_566 2_565 ? P3 Ti2 Fe1 50.43(5) 2_565 2_565 ? P3 Ti2 Fe1 105.67(6) 2 2_565 ? Fe1 Ti2 Fe1 95.05(4) 1_556 2_565 ? Fe1 Ti2 Fe1 91.68(3) 5_566 2_565 ? Fe1 Ti2 Fe1 151.39(6) 5_556 2_565 ? P3 Ti2 Fe1 50.03(4) . 2 ? P3 Ti2 Fe1 89.54(4) 5_556 2 ? P3 Ti2 Fe1 154.97(8) 5_566 2 ? P3 Ti2 Fe1 105.67(6) 2_565 2 ? P3 Ti2 Fe1 50.43(5) 2 2 ? Fe1 Ti2 Fe1 95.05(4) 1_556 2 ? Fe1 Ti2 Fe1 151.39(6) 5_566 2 ? Fe1 Ti2 Fe1 91.68(3) 5_556 2 ? Fe1 Ti2 Fe1 80.76(5) 2_565 2 ? P3 Ti2 Fe1 89.57(7) . 6_556 ? P3 Ti2 Fe1 49.73(4) 5_556 6_556 ? P3 Ti2 Fe1 49.73(4) 5_566 6_556 ? P3 Ti2 Fe1 134.22(4) 2_565 6_556 ? P3 Ti2 Fe1 134.22(4) 2 6_556 ? Fe1 Ti2 Fe1 141.29(6) 1_556 6_556 ? Fe1 Ti2 Fe1 94.48(4) 5_566 6_556 ? Fe1 Ti2 Fe1 94.48(4) 5_556 6_556 ? Fe1 Ti2 Fe1 113.86(4) 2_565 6_556 ? Fe1 Ti2 Fe1 113.86(4) 2 6_556 ? P3 Ti2 Ti2 53.55(5) . 5_556 ? P3 Ti2 Ti2 53.05(5) 5_556 5_556 ? P3 Ti2 Ti2 103.57(7) 5_566 5_556 ? P3 Ti2 Ti2 152.56(8) 2_565 5_556 ? P3 Ti2 Ti2 93.34(4) 2 5_556 ? Fe1 Ti2 Ti2 142.86(3) 1_556 5_556 ? Fe1 Ti2 Ti2 150.95(8) 5_566 5_556 ? Fe1 Ti2 Ti2 95.65(3) 5_556 5_556 ? Fe1 Ti2 Ti2 102.99(6) 2_565 5_556 ? Fe1 Ti2 Ti2 57.14(4) 2 5_556 ? Fe1 Ti2 Ti2 56.72(5) 6_556 5_556 ? Fe1 P3 Fe1 105.76(9) 2_565 2 ? Fe1 P3 Fe1 127.08(5) 2_565 . ? Fe1 P3 Fe1 127.08(5) 2 . ? Fe1 P3 Fe1 71.29(6) 2_565 6_656 ? Fe1 P3 Fe1 71.29(6) 2 6_656 ? Fe1 P3 Fe1 119.65(9) . 6_656 ? Fe1 P3 Ti2 70.61(6) 2_565 . ? Fe1 P3 Ti2 70.61(6) 2 . ? Fe1 P3 Ti2 125.84(9) . . ? Fe1 P3 Ti2 114.51(9) 6_656 . ? Fe1 P3 Ti2 142.61(10) 2_565 5_556 ? Fe1 P3 Ti2 70.69(4) 2 5_556 ? Fe1 P3 Ti2 68.99(6) . 5_556 ? Fe1 P3 Ti2 135.12(4) 6_656 5_556 ? Ti2 P3 Ti2 73.40(6) . 5_556 ? Fe1 P3 Ti2 70.69(4) 2_565 5_566 ? Fe1 P3 Ti2 142.61(10) 2 5_566 ? Fe1 P3 Ti2 68.99(6) . 5_566 ? Fe1 P3 Ti2 135.12(4) 6_656 5_566 ? Ti2 P3 Ti2 73.40(6) . 5_566 ? Ti2 P3 Ti2 89.75(7) 5_556 5_566 ? Fe1 P3 Ti2 138.88(9) 2_565 2_554 ? Fe1 P3 Ti2 68.70(4) 2 2_554 ? Fe1 P3 Ti2 69.50(6) . 2_554 ? Fe1 P3 Ti2 68.44(5) 6_656 2_554 ? Ti2 P3 Ti2 135.19(4) . 2_554 ? Ti2 P3 Ti2 76.16(3) 5_556 2_554 ? Ti2 P3 Ti2 138.48(9) 5_566 2_554 ? Fe1 P3 Ti2 68.70(4) 2_565 2_564 ? Fe1 P3 Ti2 138.88(9) 2 2_564 ? Fe1 P3 Ti2 69.50(6) . 2_564 ? Fe1 P3 Ti2 68.44(5) 6_656 2_564 ? Ti2 P3 Ti2 135.19(4) . 2_564 ? Ti2 P3 Ti2 138.48(9) 5_556 2_564 ? Ti2 P3 Ti2 76.16(3) 5_566 2_564 ? Ti2 P3 Ti2 88.88(7) 2_554 2_564 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 33.11 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.934 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.400