Investigation of thermal behavior of mixed-valent iron borates vonsenite and hulsite containing [O<i>M</i>~4~]<i>^n^</i>^+^ and [O<i>M</i>~5~]<i>^n^</i>^+^ oxocentred polyhedra by <i>in situ</i> high-temperature Mössbauer spectroscopy, X-ray diffraction and thermal analysis
Biryukov, Yaroslav P.; Zinnatullin, Almaz L.; Bubnova, Rimma S.; Vagizov, Farit G.; Shablinskii, Andrey P.; Filatov, Stanislav K.; Shilovskikh, Vladimir V.; Pekov, Igor V.; Acta Crystallographica Section B 76 (2020) 543–553; doi:10.1107/S2052520620006538

data_2108648
_publ_section_title
;
 Investigation of thermal behavior of mixed-valent iron borates vonsenite
 and hulsite containing [O<i>M</i>~4~]<i>^n^</i>^+^ and
 [O<i>M</i>~5~]<i>^n^</i>^+^ oxocentred polyhedra by <i>in situ</i>
 high-temperature M\"ossbauer spectroscopy, X-ray diffraction and thermal
 analysis
;
_journal_coeditor_code           RA5077
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              543
_journal_page_last               553
_journal_paper_doi               10.1107/S2052520620006538
_journal_volume                  76
_journal_year                    2020
_chemical_formula_sum            'B Fe2.654 Mg0.346 O5'
_chemical_formula_weight         247.4
_space_group_IT_number           55
_space_group_name_Hall           '-P 2 2ab'
_space_group_name_H-M_alt        'P b a m'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      55
_symmetry_space_group_name_Hall  '-P 2 2ab'
_symmetry_space_group_name_H-M   'P b a m'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3914(10)
_cell_length_b                   12.3034(10)
_cell_length_c                   3.0697(6)
_cell_measurement_reflns_used    404
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      0.97
_cell_volume                     354.69(8)
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            1886
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         6.61
_exptl_absorpt_coefficient_mu    10.701
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Krause et al., 2015)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.6336
_exptl_crystal_description       prizm
_exptl_crystal_F_000             473
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.02
_refine_diff_density_min         -0.81
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.82
_refine_ls_goodness_of_fit_ref   1.66
_refine_ls_number_constraints    10
_refine_ls_number_parameters     57
_refine_ls_number_reflns         404
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.0159
_refine_ls_shift/su_mean         0.0034
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0001F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0376
_refine_ls_wR_factor_ref         0.0388
_reflns_number_gt                329
_reflns_number_total             404
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ra5077sup1.cif
_cod_data_source_block           vonsenite_293K
_cod_original_formula_sum        'B1 Fe2.654 Mg0.346 O5'
_cod_database_code               2108648
_publcif_datablock.id            {44b4f208-5abd-4d8a-9c55-822d40ee089a}