Growth and Optical Properties of LixNa1-xBa12(BO3)7F4 Fluoride Borates with "Antizeolite" Structure.
Bekker, Tatyana B.; Rashchenko, Sergey V.; Solntsev, Vladimir P.; Yelisseyev, Alexander P.; Kragzhda, Alexander A.; Bakakin, Vladimir V.; Seryotkin, Yuriy V.; Kokh, Alexander E.; Kokh, Konstantin A.; Kuznetsov, Artem B.; Inorganic chemistry 56 (2017) 5411–5419; doi:10.1021/acs.inorgchem.7b00520

data_4345816
_publ_section_title
;
 Growth and Optical Properties of LixNa1-xBa12(BO3)7F4 Fluoride Borates
 with &quot;Antizeolite&quot; Structure.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5411
_journal_page_last               5419
_journal_paper_doi               10.1021/acs.inorgchem.7b00520
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'B7 Ba12 F4 Na O21'
_chemical_formula_weight         2158.74
_chemical_name_systematic        'barium sodium fluoride borate'
_space_group_crystal_system      tetragonal
_space_group_IT_number           106
_space_group_name_Hall           'P 4c -2ab'
_space_group_name_H-M_alt        'P 42 b c'
_symmetry_space_group_name_Hall  'P 4c -2ab'
_symmetry_space_group_name_H-M   'P 42 b c'
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.59612(13)
_cell_length_b                   13.59612(13)
_cell_length_c                   14.9394(3)
_cell_measurement_reflns_used    23981
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.2350
_cell_measurement_theta_min      2.0740
_cell_volume                     2761.62(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1199
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            131429
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.317
_diffrn_reflns_theta_min         2.118
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    16.925
_exptl_absorpt_correction_T_max  0.31855
_exptl_absorpt_correction_T_min  0.29724
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using 0.05 mm equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pinkish
_exptl_crystal_density_diffrn    5.192
_exptl_crystal_description       grain
_exptl_crystal_F_000             3688
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.027
_refine_diff_density_min         -2.123
_refine_diff_density_rms         0.407
_refine_ls_abs_structure_details
;
 Flack x determined using 1686 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.45(5)
_refine_ls_extinction_coef       0.00045(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         4946
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0669
_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^)+(0.0322P)^2^+127.9835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4762
_reflns_number_total             4946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00520_si_003.cif
_cod_data_source_block           shelx
_cod_database_code               4345816
_shelx_res_checksum              83238
_shelx_hkl_checksum              83604