Phase formation in the BaB2O4‒BaF2‒BaO system and new non-centrosymmetric solid-solution series Ba7(BO3)4−xF2+3x
Bekker, T. B.; Rashchenko, S. V.; Bakakin, V. V.; Seryotkin, Yu. V.; Fedorov, P. P.; Kokh, A. E.; Stonoga, S. Yu.; CrystEngComm 14 (2012) 6910–; doi:10.1039/c2ce26122g

data_7229595
_publ_contact_author_address
;Sobolev Institute of Geology and Mineralogy SB RAS
3 Academician Koptyug Av.
630090 Novosibirsk
Russian Federation
;
_publ_contact_author_email       t.b.bekker@gmail.com
_publ_contact_author_name        'Tatyana B. Bekker'
_publ_section_title
;
 Phase formation in the BaB2O4--BaF2--BaO system and new
 non-centrosymmetric solid-solution series Ba7(BO3)4&#x2212;xF2+3x
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6910
_journal_paper_doi               10.1039/c2ce26122g
_journal_volume                  14
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_sum            'B3.51 Ba7 F3.47 O10.53'
_chemical_formula_weight         1233.73
_chemical_melting_point          1030
_chemical_name_common            'Barium Fluoride Borate'
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      173
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   11.18241(11)
_cell_length_b                   11.18241(11)
_cell_length_c                   7.23720(8)
_cell_measurement_reflns_used    17040
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37.1228
_cell_measurement_theta_min      2.0987
_cell_volume                     783.740(14)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -75.00  -42.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.3125  -77.0000    0.0000 44

  2 omega  -39.00   44.25   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.3125  -77.0000    0.0000 111

  3 omega -105.00  -78.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.3125  -77.0000    0.0000 36

  4 omega  104.00  139.25   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8837  125.0000   60.0000 47

  5 omega  -31.00   -1.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8837  131.0000    2.0000 40

  6 omega   18.00  112.50   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8837 -125.0000  -90.0000 126

  7 omega   85.00  126.25   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8837  144.0000  119.0000 55

  8 omega   97.00  143.50   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8837  144.0000  -66.0000 62

  9 omega  102.00  140.25   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8837  125.0000 -180.0000 51

 10 omega   99.00  142.50   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8837  125.0000 -120.0000 58

 11 omega -143.00  -14.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5087  -77.0000  120.0000 172

 12 omega -152.00  -14.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5087  -77.0000   60.0000 184

 13 omega -143.00    2.50   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5087  -77.0000 -120.0000 194

 14 omega -150.00   -6.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5087  -77.0000 -180.0000 192

 15 omega -150.00  -12.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5087  -77.0000  -60.0000 184

 16 omega -147.00  -12.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5087  -77.0000    0.0000 180
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0563957000
_diffrn_orient_matrix_UB_12      0.0040345000
_diffrn_orient_matrix_UB_13      -0.0502103000
_diffrn_orient_matrix_UB_21      0.0360780000
_diffrn_orient_matrix_UB_22      0.0729203000
_diffrn_orient_matrix_UB_23      0.0094628000
_diffrn_orient_matrix_UB_31      0.0296218000
_diffrn_orient_matrix_UB_32      -0.0058907000
_diffrn_orient_matrix_UB_33      0.0836736000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            27864
_diffrn_reflns_theta_full        37.21
_diffrn_reflns_theta_max         37.21
_diffrn_reflns_theta_min         2.10
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    17.377
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    5.228
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1050
_exptl_crystal_recrystallization_method 'BaB2O4-BaF2-BaO system in air'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.097
_refine_diff_density_min         -2.500
_refine_diff_density_rms         0.243
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(8)
_refine_ls_extinction_coef       0.00094(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         2665
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+4.6109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0548
_reflns_number_gt                2622
_reflns_number_total             2665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Ba7NEW.cif
_cod_data_source_block           all
_cod_database_code               7229595