Cd[B2(SO4)4] and H2[B2(SO4)4] – A phyllosilicate analogue borosulfate and its homeotypic heteropolyacid
Bruns, Jörn; Höppe, Henning A.; Hämmer, Matthias; Pasqualini, Leonard C.; Huppertz, Hubert; Sebastian, Sean; Dalton Transactions  (2022) –; doi:10.1039/D2DT02344J

data_7711223
_publ_section_title
;
 Cd[B2(SO4)4] and H2[B2(SO4)4] -- A phyllosilicate analogue borosulfate
 and its homeotypic heteropolyacid
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02344J
_journal_year                    2022
_chemical_formula_sum            'B2 Cd O16 S4'
_chemical_formula_weight         518.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-05-31 deposited with the CCDC.	2022-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.959(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0611(9)
_cell_length_b                   7.9599(5)
_cell_length_c                   9.4045(10)
_cell_measurement_reflns_used    9689
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      41.26
_cell_measurement_theta_min      3.45
_cell_volume                     567.20(10)
_computing_cell_refinement       'Bruker SAINT-V 8.34A'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT-V 8.34A'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi layered optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            56664
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         41.307
_diffrn_reflns_theta_min         2.882
_diffrn_source                   'Incoatec Microfocus'
_exptl_absorpt_coefficient_mu    2.765
_exptl_absorpt_correction_T_max  0.5704
_exptl_absorpt_correction_T_min  0.4860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.035
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.0168(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         3799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_gt           0.0143
_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^)+(0.0189P)^2^+0.2186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0379
_refine_ls_wR_factor_ref         0.0386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3578
_reflns_number_total             3799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02344j2.cif
_cod_data_source_block           Cd[B2(SO4)4]
_cod_original_cell_volume        567.20(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7711223
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.648
_shelx_estimated_absorpt_t_max   0.852
_shelx_res_checksum              3741
_shelx_hkl_checksum              95207