Synthesis of Rare Earth Polyborates Using Molten Boric Acid as a Flux
Li, Linyan; Lu, Peichao; Wang, Yaoyang; Jin, Xianglin; Li, Guobao; Wang, Yingxia; You, Liping; Lin, Jianhua; Chemistry of Materials 14 (2002) 4963–4968; doi:10.1021/cm0203870

data_4000210
_publ_section_title
;
 Synthesis of Rare Earth Polyborates Using Molten Boric Acid as a Flux
;
_journal_coden_ASTM              CMATEX
_journal_issue                   12
_journal_name_full               'Chemistry of Materials'
_journal_page_first              4963
_journal_page_last               4968
_journal_paper_doi               10.1021/cm0203870
_journal_volume                  14
_journal_year                    2002
_chemical_formula_sum            'B6 Gd H3 O12'
_chemical_formula_weight         417.13
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens
;
hydrogen atoms are generated by HFIX instructions
;
_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            6
_cell_length_a                   8.405(1)
_cell_length_b                   8.405(1)
_cell_length_c                   20.771(4)
_cell_measurement_reflns_used    3228
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      3.42
_cell_volume                     1270.8(3)
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '100x100 micron'
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3228
_diffrn_reflns_theta_max         27.33
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    7.900
_exptl_absorpt_correction_T_max  1.1888
_exptl_absorpt_correction_T_min  0.7381
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.270
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1158
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.37(5)
_refine_ls_extinction_coef       0.00069(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment
;
hydrogen coordinates ride on the coordinates of the previous atom, 
the isotropic U values are 1.2 OR 1.5 time over the U values of the
previous atom.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         573
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0623
_reflns_number_gt                547
_reflns_number_total             573
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-01
;
_cod_original_sg_symbol_H-M      'R 3c'
_cod_original_formula_sum        'H3 B6 Gd O12'
_cod_database_code               4000210