Real-time synchrotron powder X-ray diffraction study of the antisite defect formation during sub- and supercritical synthesis of LiFePO~4~ and LiFe~1{-~<i>x</i>}Mn~<i>x~</i>PO~4~ nanoparticles
Jensen, Kirsten; Christensen, Mogens; Tyrsted, Christoffer; Brummerstedt Iversen, Bo; Journal of Applied Crystallography 44 (2011) 287–294; doi:10.1107/S0021889811006522

data_2300354
_publ_section_title
;
 Real-time synchrotron powder X-ray diffraction study of the antisite
 defect formation during sub- and supercritical synthesis of LiFePO~4~
 and LiFe~1{-~<i>x</i>}Mn~<i>x~</i>PO~4~ nanoparticles
;
_journal_coeditor_code           KO5132
_journal_issue                   2
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              287
_journal_page_last               294
_journal_paper_doi               10.1107/S0021889811006522
_journal_volume                  44
_journal_year                    2011
_chemical_formula_sum            'Fe0.5 Li Mn0.5 O4 P'
_chemical_name_systematic        ' ?'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   10.4072(3)
_cell_length_b                   6.06188(14)
_cell_length_c                   4.73357(13)
_cell_measurement_pressure       2.5E4
_cell_measurement_temperature    618
_cell_volume                     298.628(14)
_computing_structure_refinement  FULLPROF
_diffrn_ambient_pressure         2.5E4
_diffrn_ambient_temperature      618
_diffrn_radiation_wavelength     0.94449
_pd_block_diffractogram_id       LiFe050Mn050PO4345
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.037384
_pd_meas_2theta_range_max        43.97871
_pd_meas_2theta_range_min        3.45480
_pd_meas_number_of_points        1086
_pd_proc_2theta_range_inc        0.037384
_pd_proc_2theta_range_max        43.9655
_pd_proc_2theta_range_min        3.4416
_pd_proc_ls_pref_orient_corr     ' ?'
_pd_proc_ls_prof_R_factor        0.4143
_pd_proc_ls_prof_wR_expected     0.3334
_pd_proc_ls_prof_wR_factor       0.6095
_pd_proc_wavelength              0.944490
_pd_spec_mounting                ' ?'
_refine_ls_number_parameters     48
_refine_ls_number_reflns         175
_refine_ls_number_restraints     0
_cod_data_source_file            ko5132.cif
_cod_data_source_block           LiFe050Mn050PO4345
_cod_depositor_comments
;
Luca Lutterotti, 10/5/2013

Problem with occupancy exceeding 1.
Occupancy corrected using following rules:
- Fe/Mn and Li relatives occupancies as refined by authors
- Fe/Mn ratio fixed to nominal composition: 0.75/0.25, 0.5/0.5, 0.25/0.75
- O and P occupancies = 1
Everything turn out correct this way.

 The original ko5132.cif from the IUCr web-site was updated according
 to the message received from the authors:

 From:  Bo Brummerstedt Iversen <bo@xxxxxxxxxxxxxxxxx>
 To:    Saulius Gra\<ulis <grazulis@xxxxxxxxxxxxxxx>
 Subject:        Re: Supplementary data for your paper ko5132.cif
 Date:           Thu, 12 May 2011 10:27:02 +0200 (11:27 EEST)

 Dear Saulius,

 Thanks for your mail

 1) /.../ The compositions are LiFePO4, LiFe0.75Mn0.25PO4,
 LiFe0.50Mn0.50PO4, and LiFe0.25Mn0.50PO4

 The occupancy of the Fe in the second block should therefore be
 changed to 0.7465(17), while that of manganese should be 0.25096. We
 are sorry about this confusion.

 2) Yes, the bruttoformula should be the data header, and the Z value 4

 3) Yes, the data were measured at 345 degrees celcius.

 4) Yes, the pressure during the measurement was 250 bar.
 /.../

 Best regards,
 Bo

 Saulius Gra\<zulis
 2011.05.17

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        298.629(14)
_cod_original_formula_sum        'Li Fe0.50 Mn0.50 P O4'
_cod_database_code               2300354