Time-Retrenched Synthesis of BaTaO2N by Localizing an NH3 Delivery System for Visible-Light-Driven Photoelectrochemical Water Oxidation at Neutral pH: Solid-State Reaction or Flux Method?
Hojamberdiev, Mirabbos; Mora-Hernandez, J. Manuel; Vargas, Ronald; Yamakata, Akira; Yubuta, Kunio; Heppke, Eva Maria; Torres-Martínez, Leticia M.; Teshima, Katsuya; Lerch, Martin; ACS Applied Energy Materials 4 (2021) 9315–9327; doi:10.1021/acsaem.1c01539

data_4519032
_publ_section_title
;
 Time-Retrenched Synthesis of BaTaO2N by Localizing an NH3 Delivery System
 for Visible-Light-Driven Photoelectrochemical Water Oxidation at Neutral
 pH: Solid-State Reaction or Flux Method?
;
_journal_issue                   9
_journal_name_full               'ACS Applied Energy Materials'
_journal_page_first              9315
_journal_page_last               9327
_journal_paper_doi               10.1021/acsaem.1c01539
_journal_volume                  4
_journal_year                    2021
_chemical_compound_source        synthetic
_chemical_formula_iupac          'Ba Ta O2.42 N0.58'
_chemical_formula_structural     'Ba Ta O2.42 N0.58'
_chemical_formula_sum            'Ba N0.58 O2.42 Ta'
_chemical_formula_weight         365.130334
_chemical_name_common            'barium tantalum oxynitride'
_chemical_name_systematic        'barium tantalum dioxide nitride'
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 4 2 3'
_symmetry_space_group_name_H-M   'P m -3 m'
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            1
_cell_length_a                   4.11158(6)
_cell_length_b                   4.11158(6)
_cell_length_c                   4.11158(6)
_cell_measurement_temperature    293
_cell_volume                     69.5066(18)
_computing_cell_refinement       'FullProf (Rodr\'iguez-Carvajal, 1993)'
_computing_data_collection       'X'Pert Data Collector (PANalytical, 2008)'
_computing_data_reduction        'X'Pert Data Collector (PANalytical, 2008)'
_computing_molecular_graphics    'Diamond (Brandenburg, 2013)'
_computing_publication_material  'WinPLOTR (Roisnel, 2001)'
_computing_structure_refinement  'FULLPROF (Rodr\'iguez-Carvajal, 1993)'
_computing_structure_solution    'ICSD (Bergerhoff, 1987)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'solid-state RTMS detector'
_diffrn_detector_type            'PANalytical PIXcel'
_diffrn_measurement_device       '\q-\q geometry diffractometer'
_diffrn_measurement_device_type  'PANalytical X'Pert Pro'
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Philips PW3373-10'
_exptl_absorpt_coefficient_mu    178.873
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
roughness/microabsorption correction according to Pitschke, Hermann, and
Mattern (Pitschke et al., 1993):  P~0~ = 0.708(10), C = 1.9224, \t = 0.0101
;
_exptl_crystal_density_diffrn    8.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       powder
_exptl_crystal_F_000             152
_pd_calc_method                  'Rietveld refinement'
_pd_char_colour                  red
_pd_instr_geometry               Bragg-Brentano
_pd_meas_2theta_range_inc        0.026008
_pd_meas_2theta_range_max        119.96713
_pd_meas_2theta_range_min        10.16913
_pd_meas_number_of_points        4224
_pd_meas_scan_method             step
_pd_proc_2theta_range_inc        0.026008
_pd_proc_2theta_range_max        119.9671
_pd_proc_2theta_range_min        10.1691
_pd_proc_ls_background_function
;
linear interpolation between 18 manually defined background points
with refined heights
;
_pd_proc_ls_peak_cutoff          0.005
_pd_proc_ls_profile_function
;
pseudo-Voigt function with U = 0.299(11), V = -0.0146(131), W = 0.0234(4), 
\h~0~ = 0.460(13), X = 0.0031(2),
asymmetry correction (whole profile):
A~S~(z) = 1+[P~1~F~a~(z)+P~2~F~b~(z)]/tanh(\q~h~)
with P~1~ = 0.0127(6), P~2~ = 0.0445(12)
;
_pd_proc_ls_prof_R_factor        0.020239
_pd_proc_ls_prof_wR_expected     0.017972
_pd_proc_ls_prof_wR_factor       0.028232
_pd_proc_number_of_points        4224
_pd_proc_wavelength              1.540560
_pd_spec_mounting                'drifted powder on off-cut Si'
_pd_spec_mount_mode              reflection
_pd_spec_size_axial              10
_pd_spec_size_thick              0.2
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.57
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    1
_refine_ls_number_parameters     32
_refine_ls_number_reflns         44
_refine_ls_number_restraints     0
_refine_ls_R_I_factor            0.014299
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0248
_cod_data_source_file            ae1c01539_si_002.cif
_cod_data_source_block           BaTaO2Nflux
_cod_original_cell_volume        69.5065(16)
_cod_database_code               4519032
_pd_proc_ls_prof_cr_factor       0.092337
_pd_proc_ls_prof_cwr_factor      0.066578
_pd_proc_ls_prof_cwr_expected    0.042384
_pd_proc_ls_prof_chi2            2.4675
_pd_proc_ls_prof_echi2           3.1469