New KRb2Sb4BO13 and Rb3Sb4BO13 compounds prepared by Rb+/K+ ion exchange from the K3Sb4BO13 ion conductor
Doux, Jean-Marie; Stephant, Nicolas; La Salle, Annie Le Gal; Joubert, Olivier; Guyomard, Dominique; Quarez, Eric; CrystEngComm 21 (2019) 594–; doi:10.1039/C8CE01712C

data_7231901
_publ_section_title
;
 New KRb2Sb4BO13 and Rb3Sb4BO13 compounds prepared by Rb+/K+ ion exchange
 from the K3Sb4BO13 ion conductor
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              594
_journal_paper_doi               10.1039/C8CE01712C
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'B K3 O13 Sb4'
_chemical_formula_weight         823.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-10-02 deposited with the CCDC.
2018-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                81.973(3)
_cell_angle_beta                 99.788(4)
_cell_angle_gamma                117.046(4)
_cell_formula_units_Z            2
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_cell_length_b                   7.2147(3)
_cell_length_c                   13.2268(4)
_cell_measurement_reflns_used    10952
_cell_measurement_temperature    295
_cell_measurement_theta_max      36.394
_cell_measurement_theta_min      1.566
_cell_volume                     594.55(5)
_computing_cell_refinement       'Dirax/LSQ (Duisenberg et al., 2000)'
_computing_data_collection       'Collect (Nonius BV, 1998)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10952
_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         36.394
_diffrn_reflns_theta_min         1.566
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    10.112
_exptl_absorpt_correction_T_max  0.5684
_exptl_absorpt_correction_T_min  0.1619
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_exptl_absorpt_process_details   Jana2006
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.598
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.354
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_exptl_crystal_size_min          0.102
_refine_diff_density_max         2.911
_refine_diff_density_min         -1.897
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_refine_ls_extinction_coef       0.00333(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         5787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0372
_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^)+6.1913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4749
_reflns_number_total             5787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01712c1.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7231901--7231903.cif.'
_cod_database_code               7231901
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              60032