Synthesis, Characterization, and Crystal Structure of a New Trisodium Triborate, Na3[B3O4(OH)4]
Jérôme Andrieux; Christelle Goutaudier; Laetitia Laversenne; Erwann Jeanneau; Philippe Miele; Inorganic Chemistry 49 (2010) 4830–4835; doi:10.1021/ic902525s

data_4315732
_publ_section_title
;
 Synthesis, Characterization, and Crystal Structure of a New Trisodium
 Triborate, Na3[B3O4(OH)4]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4830
_journal_page_last               4835
_journal_paper_doi               10.1021/ic902525s
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'H4 B3 Na3 O8'
_chemical_formula_sum            'B3 H4 Na3 O8'
_chemical_formula_weight         233.43
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-02-03
_audit_creation_method           CRYSTALS_ver_12.85
_audit_update_record
;
2009-12-17 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 98.161(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8274(6)
_cell_length_b                   7.7276(4)
_cell_length_c                   6.9690(3)
_cell_measurement_reflns_used    729
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.730
_cell_volume                     683.81(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.016
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1443
_diffrn_reflns_theta_full        27.291
_diffrn_reflns_theta_max         27.848
_diffrn_reflns_theta_min         3.086
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.9289
_exptl_absorpt_correction_T_min  0.9221
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.20
_refine_diff_density_min         -0.21
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.7(6)
_refine_ls_extinction_coef       710(20)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9679
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         808
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.000307
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.890 0.153 0.566 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0239
_refine_ls_wR_factor_gt          0.0238
_refine_ls_wR_factor_ref         0.0239
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                802
_reflns_number_total             810
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0204
_oxford_refine_ls_scale          1.053(4)
_oxford_reflns_number_all        808
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic902525s_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

2021-05-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'C 1 c 1 '
_cod_original_formula_moiety     'H8 B6 Na6 O16'
_cod_original_formula_sum        'H8 B6 Na6 O16'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     466.86
_cod_database_code               4315732