Synthesis, crystal structure and possible proton conduction of Fe(H2PO4)2F
Ma, Zihan; Lander, Laura; Nishimura, Shin-ichi; Fukakusa, Chihoko; Yamada, Teppei; Okubo, Masashi; Yamada, Atsuo; Solid State Ionics 338 (2019) 134–; doi:10.1016/j.ssi.2019.05.019

data_1551894
_publ_section_title
;
 Synthesis, crystal structure and possible proton conduction of
 Fe(H2PO4)2F
;
_journal_name_full               'Solid State Ionics'
_journal_page_first              134
_journal_paper_doi               10.1016/j.ssi.2019.05.019
_journal_volume                  338
_journal_year                    2019
_chemical_formula_moiety         '0.25(F4 Fe4 H16 O32 P8)'
_chemical_formula_sum            'F Fe H4 O8 P2'
_chemical_formula_weight         268.82
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_contact_author_name       'Shinichi Nishimura '
_audit_creation_date             2018-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.01870(10)
_cell_length_b                   9.01870(10)
_cell_length_c                   7.8058(2)
_cell_measurement_reflns_used    4144
_cell_measurement_temperature    295
_cell_measurement_theta_max      32.4680
_cell_measurement_theta_min      3.1850
_cell_volume                     634.900(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      295
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'AFC12 (Right): 1/4 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen Dual Thickness McroMounts 100um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0073
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4638
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         30.457
_diffrn_reflns_theta_min         3.194
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.913
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.63290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
_computing_data_collection     'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement     'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction      'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
;
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.812
_exptl_crystal_description       block
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.296
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         283
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.395
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.8963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                283
_reflns_number_total             283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            FeHPOF_20180611_01_298K_.cif
_cod_data_source_block           fehpof_20180611_01_298k_
_cod_original_cell_volume        634.90(2)
_cod_database_code               1551894
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Restrained distances
 O2-H2_$1
 0.98 with sigma of 0.02
 H2_$1-P1
 1.9 with sigma of 0.04
2. Others
 Fixed Sof: H2(0.5)
;