Hydrothermal synthesis and structural analysis of new mixed oxyanion borates: Ba11B26O44(PO4)2(OH)6, Li9BaB15O27(CO3) and Ba3Si2B6O16
Heyward, Carla; McMillen, Colin D.; Kolis, Joseph; Journal of Solid State Chemistry 203 (2013) 166–173; doi:10.1016/j.jssc.2013.04.022

data_1562609
_publ_section_title
;
 Hydrothermal synthesis and structural analysis of new mixed oxyanion
 borates: Ba11B26O44(PO4)2(OH)6, Li9BaB15O27(CO3) and Ba3Si2B6O16
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              166
_journal_page_last               173
_journal_paper_doi               10.1016/j.jssc.2013.04.022
_journal_volume                  203
_journal_year                    2013
_chemical_formula_sum            'C B15 Ba Li9 O30'
_chemical_formula_weight         853.96
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   8.8599(13)
_cell_length_b                   8.8599(13)
_cell_length_c                   15.148(3)
_cell_measurement_reflns_used    5895
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.3272
_cell_measurement_theta_min      2.6531
_cell_volume                     1029.8(3)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 1999)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker-AXS, 1999)'
_computing_publication_material  'SHELXTL (Bruker-AXS, 1999)'
_computing_structure_refinement  'SHELXTL (Bruker-AXS, 1999)'
_computing_structure_solution    'SHELXTL (Bruker-AXS, 1999)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC8S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9201
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.089
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB, CrystalClear'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.0231(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    .
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+0.8587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0554
_reflns_number_gt                686
_reflns_number_total             702
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2013-203-166.cif
_cod_data_source_block           252hex
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Trigonal' was changed to
'trigonal' in accordance with the built-in table derived from the CIF
Core dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_sg_symbol_H-M      P-31c
_cod_database_code               1562609