Syntheses, structure determination and characterization of two novel non-centrosymmetric mixed alkali rare-earth orthoborates: K3Li3RE7(BO3)9 (RE=Dy, Tb)
Chen, P.Y.; Wang, Guirong; Solid State Sciences 108 (2020) 106442–; doi:10.1016/j.solidstatesciences.2020.106442

data_1559842
_publ_section_title
;
 Syntheses, structure determination and characterization of two novel
 non-centrosymmetric mixed alkali rare-earth orthoborates: K3Li3RE7(BO3)9
 (RE=Dy, Tb)
;
_journal_name_full               'Solid State Sciences'
_journal_page_first              106442
_journal_paper_doi               10.1016/j.solidstatesciences.2020.106442
_journal_volume                  108
_journal_year                    2020
_chemical_formula_sum            'B9 K3 Li3 O27 Tb7'
_chemical_formula_weight         1779.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   .
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9218(9)
_cell_length_b                   6.4420(3)
_cell_length_c                   17.5285(8)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      3.03
_cell_volume                     2362.46(18)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku XtaLAB AFC12'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            132110
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.615
_diffrn_reflns_theta_min         1.947
_exptl_absorpt_coefficient_mu    21.316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'North et al., 1968'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.004
_exptl_crystal_description       prism
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_transmission_factor_max   0.20
_exptl_transmission_factor_min   0.10
_refine_diff_density_max         1.022
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.224
_refine_ls_abs_structure_details
;
 Flack x determined using 3169 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(6)
_refine_ls_extinction_coef       0.000847(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         7278
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0069P)^2^+8.4259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0305
_refine_ls_wR_factor_ref         0.0313
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6890
_reflns_number_total             7278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            K3Li3Tb7BO39-Cod.cif
_cod_data_source_block           K3Li3Tb7B9O27
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' 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_database_code               1559842
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              42676