#------------------------------------------------------------------------------ #$Date: 2025-07-01 14:20:32 +0300 (Tue, 01 Jul 2025) $ #$Revision: 1228 $ #$URL: svn://localhost/testcod/cif/4/00/00/4000032.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000032 loop_ _publ_author_name 'Song, Yanning' 'Zavalij, Peter Y.' 'Chernova, Natasha A.' 'Whittingham, M. Stanley' _publ_section_title ; Synthesis, Crystal Structure, and Electrochemical and Magnetic Study of New Iron (III) Hydroxyl-Phosphates, Isostructural with Lipscombite ; _journal_issue 5 _journal_name_full 'Chemistry of Materials' _journal_page_first 1139 _journal_page_last 1147 _journal_paper_doi 10.1021/cm049406r _journal_volume 17 _journal_year 2005 _chemical_formula_moiety 'Fe1.375 O5 P' _chemical_formula_structural Fe1.375(PO4)(OH) _chemical_formula_sum 'Fe1.375 O5 P' _chemical_formula_weight 187.77 _chemical_name_common 'Iron phosphate hydroxide' _space_group_IT_number 141 _space_group_name_Hall '-I 4bd 2' _space_group_name_H-M_alt 'I 41/a m d :2' _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-I 4bd 2' _symmetry_space_group_name_H-M 'I 41/a m d :2' _audit_creation_date 2003-09-03T14:02 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_update_record ; 2003-09-03T14:02 Initial CIF as created by GSAS2CIF 2004-04-09T00:40 Edited ; _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_formula_units_Z 4 _cell_length_a 5.19183(12) _cell_length_b 5.19183(12) _cell_length_c 12.9927(4) _cell_measurement_temperature 295 _cell_volume 350.220(16) _computing_data_collection 'DMSNT (1999)' _computing_molecular_graphics 'ATOMS (Dowty, 1999)' _computing_publication_material 'EXPGUI (Toby, 2001)' _computing_structure_refinement 'GSAS (Larson & Von Dreele, 2000)' _diffrn_ambient_temperature 295 _diffrn_detector 'Ge(Li) solid state' _diffrn_detector_type 'solid state' _diffrn_measurement_device_type 'Scintag XDS2000 powder diffractometer' _diffrn_radiation_polarisn_ratio 0.5 _diffrn_radiation_probe X-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_number 49 _diffrn_reflns_theta_max 44.9 _diffrn_reflns_theta_min 9.2 _diffrn_source 'sealed X-ray tube' _diffrn_source_target Cu _exptl_absorpt_coefficient_mu 50.0 _exptl_absorpt_correction_T_max 0.96520 _exptl_absorpt_correction_T_min 0.75527 _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 3 Surface roughness abs. correction (Suortti) Terms = 0.62927 0.32678 ; _exptl_crystal_density_diffrn 3.561 _exptl_crystal_density_meas 3.513 _exptl_crystal_density_method 'gas replacement' _exptl_crystal_F_000 362.7 _pd_block_id 2003-09-03T14:02|_HTL0304SLW|Song_Yanning|scintag _pd_calc_method 'Rietveld Refinement' _pd_char_colour yellow _pd_char_particle_morphology plate-like _pd_instr_geometry Bragg-Brentano _pd_meas_2theta_range_inc 0.02 _pd_meas_2theta_range_max 89.98 _pd_meas_2theta_range_min 17.02 _pd_meas_number_of_points 3649 _pd_meas_scan_method step _pd_phase_name Fe133 _pd_prep_temperature 295 _pd_proc_2theta_range_inc 0.02 _pd_proc_2theta_range_max 89.98 _pd_proc_2theta_range_min 17.02 _pd_proc_info_datetime 2003-09-03T14:02:51 _pd_proc_ls_background_function ; GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind ; _pd_proc_ls_peak_cutoff 0.00200 _pd_proc_ls_profile_function ; CW Profile function number 4 with 16 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. Microstrain broadening by P.W. Stephens, (1999). J. Appl. Cryst.,32,281-289. Peak tails are ignored where the intensity is below 0.0020 times the peak ; _pd_proc_ls_prof_R_factor 0.0912 _pd_proc_ls_prof_wR_expected 0.0929 _pd_proc_ls_prof_wR_factor 0.1256 _pd_proc_number_of_points 3649 _pd_spec_mounting 'packed powder pellet' _pd_spec_mount_mode reflection _pd_spec_shape flat-sheet _pd_spec_size_axial 25 _pd_spec_size_equat 25 _pd_spec_size_thick 1 _refine_ls_goodness_of_fit_all 1.36 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 30 _refine_ls_number_restraints 0 _refine_ls_R_Fsqd_factor 0.06925 _refine_ls_shift/su_max 0.07 _refine_ls_shift/su_mean 0.02 _refine_ls_structure_factor_coef Inet _refine_ls_weighting_scheme calc _reflns_d_resolution_high 1.093 _reflns_d_resolution_low 4.821 _reflns_limit_h_max 4 _reflns_limit_h_min 0 _reflns_limit_k_max 4 _reflns_limit_k_min 0 _reflns_limit_l_max 11 _reflns_limit_l_min 0 _reflns_number_gt 49 _reflns_number_total 49 _cod_data_source_file cm049406rsi20040409_102223.cif _cod_data_source_block '_Fe133' _cod_original_cell_volume 350.22(1) _cod_original_sg_symbol_H-M 'I 41/a m d' _cod_database_code 4000032 _pd_instr_const_illum_flag no loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -y+1/4,+x+3/4,+z+1/4 3 -x+1/2,-y,+z+1/2 4 +y+1/4,-x+1/4,+z+3/4 5 -x,+y,+z 6 -y+1/4,-x+3/4,+z+1/4 7 +x+1/2,-y,+z+1/2 8 +y+1/4,+x+1/4,+z+3/4 -1 -x,-y,-z -2 +y+3/4,-x+1/4,-z+3/4 -3 +x+1/2,+y,-z+1/2 -4 -y+3/4,+x+3/4,-z+1/4 -5 +x,-y,-z -6 +y+3/4,+x+1/4,-z+3/4 -7 -x+1/2,+y,-z+1/2 -8 -y+3/4,-x+3/4,-z+1/4 101 +x+1/2,+y+1/2,+z+1/2 102 -y+3/4,+x+1/4,+z+3/4 103 -x,-y+1/2,+z 104 +y+3/4,-x+3/4,+z+1/4 105 -x+1/2,+y+1/2,+z+1/2 106 -y+3/4,-x+1/4,+z+3/4 107 +x,-y+1/2,+z 108 +y+3/4,+x+3/4,+z+1/4 -101 -x+1/2,-y+1/2,-z+1/2 -102 +y+1/4,-x+3/4,-z+1/4 -103 +x,+y+1/2,-z -104 -y+1/4,+x+1/4,-z+3/4 -105 +x+1/2,-y+1/2,-z+1/2 -106 +y+1/4,+x+3/4,-z+1/4 -107 -x,+y+1/2,-z -108 -y+1/4,-x+1/4,-z+3/4 loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity P P1 0.0 0.75 0.125 1.0 Uiso 0.0134(8) 4 O O1 0.0 0.5045(5) 0.19024(22) 1.0 Uiso 0.0264(11) 16 O O2 0.0 0.25 0.375 1.0 Uiso 0.0142(18) 4 FE Fe1 0.0 0.0420(5) 0.4939(4) 0.3438(9) Uiso 0.0166(5) 16 loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source P 4.0 0.283 0.434 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080 68.1645 1.11490 International_Tables_Vol_C FE 5.501 -1.179 3.204 11.7695 4.76110 7.35730 0.30720 3.52220 15.3535 2.30450 76.8805 1.03690 International_Tables_Vol_C O 20.0 0.047 0.032 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 P1 O1 107.86(10) 1_555 . -4_666 Y O1 P1 O1 112.75(21) 1_555 . 103_565 Y O1 P1 O1 107.86(10) 1_555 . -102_566 Y O1 P1 O1 107.86(10) -4_666 . 103_565 Y O1 P1 O1 112.75(21) -4_666 . -102_566 Y O1 P1 O1 107.86(10) 103_565 . -102_566 Y P1 O1 Fe1 134.30(9) 1_555 . 4_554 N P1 O1 Fe1 145.54(9) 1_555 . -2_566 N Fe1 O1 Fe1 80.01(10) 4_554 . -2_566 N Fe1 O1 Fe1 90.83(17) 4_554 . 102_454 N Fe1 O1 Fe1 11.63(19) 4_554 . -104_566 N Fe1 O1 Fe1 68.91(18) -2_566 . -104_566 N Fe1 O2 Fe1 132.20(14) 1_555 . -2_566 N Fe1 O2 Fe1 69.92(22) 1_555 . 103_464 N O1 Fe1 O1 168.37(19) 2_545 . -2_566 N O1 Fe1 O1 76.75(16) 2_545 . 104_545 N O1 Fe1 O1 96.90(13) 2_545 . -104_657 N O1 Fe1 O2 98.03(19) 2_545 . 1_555 N O1 Fe1 O1 96.90(13) -2_566 . 104_545 N O1 Fe1 O1 87.59(21) -2_566 . -104_657 N O1 Fe1 O2 92.47(13) -2_566 . 1_555 N O1 Fe1 O1 168.37(19) 104_545 . -104_657 N O1 Fe1 O2 98.03(19) 104_445 . 1_555 N O1 Fe1 O2 92.47(13) -104_557 . 1_555 N loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O1 1.531(3) . 1_555 Y P1 O1 1.531(3) . -4_666 Y P1 O1 1.531(3) . 103_565 Y P1 O1 1.531(3) . -102_455 Y Fe1 O1 2.128(3) . 2_545 N Fe1 O1 1.909(3) . -2_566 N Fe1 O1 2.128(3) . 104_445 N Fe1 O1 1.909(3) . -104_555 N Fe1 O2 1.885(4) . 1_555 N Fe1 O2 2.280(4) . 2_545 N Fe1 Fe1 2.160(6) . 103_555 N Fe1 Fe1 2.6007(6) . -103_455 N loop_ _refln_index_h _refln_index_k _refln_index_l _pd_refln_wavelength_id _refln_observed_status _refln_F_squared_meas _refln_F_squared_calc _refln_phase_calc _refln_d_spacing _gsas_i100_meas 1 0 1 1 o 734.776 676.195 180.00 4.82116 9.39 1 0 1 2 o 725.062 676.195 180.00 4.82116 4.59 1 0 3 1 o 13514.853 13065.608 180.00 3.32571 100.00 1 0 3 2 o 13383.789 13065.608 180.00 3.32571 49.26 0 0 4 1 o 2460.672 2606.078 0.00 3.24817 3.60 0 0 4 2 o 2520.549 2606.078 0.00 3.24817 1.85 1 1 2 1 o 5300.838 5406.800 0.00 3.19613 38.54 1 1 2 2 o 5285.547 5406.800 0.00 3.19613 19.12 2 0 0 1 o 5712.844 4862.127 0.00 2.59592 13.48 2 0 0 2 o 5842.513 4862.127 0.00 2.59592 6.85 2 0 2 1 o 1984.751 1358.998 0.00 2.41058 7.10 2 0 2 2 o 1993.186 1358.998 0.00 2.41058 3.55 1 0 5 1 o 814.236 771.299 180.00 2.32373 2.76 1 0 5 2 o 777.737 771.299 180.00 2.32373 1.30 2 1 1 1 o 1678.241 1777.007 0.00 2.28565 11.11 2 1 1 2 o 1591.400 1777.007 0.00 2.28565 5.22 2 1 3 1 o 3840.906 3769.903 180.00 2.04633 19.59 2 1 3 2 o 3866.232 3769.903 180.00 2.04633 9.81 2 0 4 1 o 2221.061 2218.831 180.00 2.02787 6.48 2 0 4 2 o 2234.014 2218.831 180.00 2.02787 3.24 1 1 6 1 o 2291.305 1902.697 180.00 1.86516 5.49 1 1 6 2 o 2258.578 1902.697 180.00 1.86516 2.70 2 2 0 1 o 8000.631 7664.685 0.00 1.83559 7.85 2 2 0 2 o 8171.986 7664.685 0.00 1.83559 4.00 1 0 7 1 o 2002.374 1692.300 180.00 1.74777 3.51 1 0 7 2 o 1951.928 1692.300 180.00 1.74777 1.69 2 1 5 1 o 48.028 29.529 180.00 1.73139 0.46 2 1 5 2 o 38.631 29.529 180.00 1.73139 0.21 3 0 1 1 o 487.782 435.182 180.00 1.71546 0.74 3 0 1 2 o 435.982 435.182 180.00 1.71546 0.32 2 0 6 1 o 11550.313 11706.229 0.00 1.66285 18.68 2 0 6 2 o 11487.868 11706.229 0.00 1.66285 9.23 0 0 8 1 o 5368.870 4847.997 0.00 1.62409 2.05 0 0 8 2 o 5602.725 4847.997 0.00 1.62409 1.07 3 0 3 1 o 6465.775 6161.873 180.00 1.60705 10.00 3 0 3 2 o 6102.052 6161.873 180.00 1.60705 4.68 2 2 4 1 o 12654.175 13346.007 0.00 1.59807 19.12 2 2 4 2 o 12521.110 13346.007 0.00 1.59807 9.40 3 1 2 1 o 1658.614 1765.403 0.00 1.59175 5.56 3 1 2 2 o 1734.891 1765.403 0.00 1.59175 2.89 3 1 4 1 o 1.169 8.337 0.00 1.46526 0.00 3 1 4 2 o 19.966 8.337 0.00 1.46526 0.02 2 1 7 1 o 3191.128 2950.426 180.00 1.44979 7.77 2 1 7 2 o 3341.572 2950.426 180.00 1.44979 4.05 3 0 5 1 o 601.472 413.383 180.00 1.44040 0.72 3 2 1 1 o 1118.483 1123.027 180.00 1.43119 2.57 3 0 5 2 o 565.030 413.383 180.00 1.44040 0.33 3 2 1 2 o 1024.562 1123.027 180.00 1.43119 1.17 1 0 9 1 o 816.640 892.745 180.00 1.39086 0.78 1 0 9 2 o 919.871 892.745 180.00 1.39086 0.45 2 0 8 1 o 1969.702 1887.664 0.00 1.37683 2.31 2 0 8 2 o 1885.160 1887.664 0.00 1.37683 1.10 3 2 3 1 o 1034.732 1065.209 180.00 1.36641 2.01 3 2 3 2 o 1108.106 1065.209 180.00 1.36641 1.08 3 1 6 1 o 2084.208 1708.658 180.00 1.30829 4.37 3 1 6 2 o 2076.497 1708.658 180.00 1.30829 2.16 4 0 0 2 o 15564.437 14817.577 0.00 1.29796 3.75 4 0 0 1 o 15951.869 14817.577 0.00 1.29796 7.73 4 0 2 1 o 283.648 250.017 0.00 1.27280 0.24 4 0 2 2 o 264.066 250.017 0.00 1.27280 0.11 3 0 7 1 o 1008.981 1053.177 180.00 1.26577 0.80 3 0 7 2 o 984.708 1053.177 180.00 1.26577 0.39 3 2 5 1 o 15.669 12.086 180.00 1.25950 0.07 3 2 5 2 o 8.740 12.086 180.00 1.25950 0.03 4 1 1 1 o -4.568 4.494 0.00 1.25333 0.03 4 1 1 2 o -9.575 4.494 0.00 1.25333 0.01 2 1 9 1 o 1283.510 1305.599 0.00 1.22598 2.18 1 1 10 1 o 1587.268 1610.705 0.00 1.22483 1.46 2 1 9 2 o 1289.464 1305.599 0.00 1.22598 1.09 1 1 10 2 o 1603.736 1610.705 0.00 1.22483 0.73 2 2 8 1 o 386.648 317.581 180.00 1.21634 0.64 2 2 8 2 o 352.269 317.581 180.00 1.21634 0.30 4 1 3 1 o 1630.568 1502.126 0.00 1.20913 2.80 3 3 2 1 o 845.302 846.870 180.00 1.20258 0.79 4 1 3 2 o 1615.349 1502.126 0.00 1.20913 1.38 4 0 4 1 o 141.048 132.872 0.00 1.20529 0.11 3 3 2 2 o 811.928 846.870 180.00 1.20258 0.38 4 0 4 2 o 132.712 132.872 0.00 1.20529 0.05 2 0 10 1 o 5838.964 5368.586 0.00 1.16187 4.39 4 2 0 1 o 544.830 501.617 180.00 1.16093 0.52 2 0 10 2 o 5622.707 5368.586 0.00 1.16187 2.10 4 2 0 2 o 528.338 501.617 180.00 1.16093 0.25 1 0 11 1 o 646.944 433.813 180.00 1.15172 0.50 3 1 8 1 o 75.573 63.310 0.00 1.15461 0.11 1 0 11 2 o 612.960 433.813 180.00 1.15172 0.23 3 1 8 2 o 96.185 63.310 0.00 1.15461 0.07 4 2 2 1 o 361.009 259.249 0.00 1.14282 0.53 4 2 2 2 o 331.341 259.249 0.00 1.14282 0.24 3 2 7 1 o 1573.434 1314.287 180.00 1.13772 2.42 3 2 7 2 o 1452.373 1314.287 180.00 1.13772 1.11 4 1 5 1 o 143.105 132.847 180.00 1.13317 0.22 4 1 5 2 o 105.213 132.847 180.00 1.13317 0.08 4 0 6 1 o 141.807 173.478 0.00 1.11329 0.09 4 0 6 2 o 185.769 173.478 0.00 1.11329 0.06 3 0 9 1 o 101.873 107.458 180.00 1.10857 0.06 3 0 9 2 o 98.200 107.458 180.00 1.10857 0.03 4 2 4 1 o 1830.462 1619.630 0.00 1.09320 2.79 4 2 4 2 o 1774.968 1619.630 0.00 1.09320 1.35