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_1562610
_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            'B26 Ba11 H6 O58 P2'
_chemical_formula_weight         2787.79
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.8909(14)
_cell_length_b                   13.629(3)
_cell_length_c                   25.581(5)
_cell_measurement_reflns_used    10899
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.0265
_cell_measurement_theta_min      2.8163
_cell_volume                     2402.5(9)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 1999)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 1999)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0855
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            21920
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.076
_exptl_absorpt_correction_T_max  0.7724
_exptl_absorpt_correction_T_min  0.3245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB, CrystalClear'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.854
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.980
_refine_diff_density_min         -2.103
_refine_diff_density_rms         0.365
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         4731
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0588P)^2^+11.7110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1402
_reflns_number_gt                3759
_reflns_number_total             4731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2013-203-166.cif
_cod_data_source_block           454n
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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_cell_volume        2402.5(8)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1562610