High-temperature, high-pressure hydrothermal synthesis, crystal structure, and solid state NMR spectroscopy of a lead borosilicate with boron-silicon mixing: Pb<sub>6</sub>B<sub>2</sub>Si<sub>8</sub>O<sub>25</sub>.
Chang, Ling-Wei; Lii, Kwang-Hwa; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11173–11179; doi:10.1039/d1dt02027g

data_7707937
_publ_section_title
;
 High-temperature, high-pressure hydrothermal synthesis, crystal
 structure, and solid state NMR spectroscopy of a lead borosilicate with
 boron-silicon mixing:
 Pb<sub>6</sub>B<sub>2</sub>Si<sub>8</sub>O<sub>25</sub>.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11173
_journal_page_last               11179
_journal_paper_doi               10.1039/d1dt02027g
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'B2 O25 Pb6 Si8'
_chemical_formula_weight         1889.48
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-06-14 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   9.5090(2)
_cell_length_b                   9.5090(2)
_cell_length_c                   42.3552(8)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.65
_cell_volume                     3316.71(12)
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Bruker D8 QUEST CMOS PHOTON II four-circle KAPPA'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            17373
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.292
_diffrn_reflns_theta_min         2.654
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    46.077
_exptl_absorpt_correction_type   'Numerical Mu Calculated'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.676
_exptl_crystal_description       lamellar
_exptl_crystal_F_000             4884
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.039
_exptl_transmission_factor_max   0.2812
_exptl_transmission_factor_min   0.0215
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       0.000033(4)
_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   1.126
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0147
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+44.8389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0301
_refine_ls_wR_factor_ref         0.0309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                851
_reflns_number_total             928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02027g2.cif
_cod_data_source_block           PbBSiO
_cod_depositor_comments          'Adding full bibliography for 7707937.cif.'
_cod_original_cell_volume        3316.70(15)
_cod_database_code               7707937
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              6717