Pb4(BO3)2(SO4) and Pb2[(BO2)(OH)](SO4): New lead(II) borate-sulfate mixed-anion compounds with two types of 3D network structures
Ruan, Ting-Ting; Wang, Wen-Wen; Hu, Chun-Li; Xu, Xiang; Mao, Jiang-Gao; Journal of Solid State Chemistry 260 (2018) 39–45; doi:10.1016/j.jssc.2018.01.013

data_1561146
_publ_section_title
;
 Pb4(BO3)2(SO4) and Pb2[(BO2)(OH)](SO4): New lead(II) borate-sulfate
 mixed-anion compounds with two types of 3D network structures
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              39
_journal_page_last               45
_journal_paper_doi               10.1016/j.jssc.2018.01.013
_journal_volume                  260
_journal_year                    2018
_chemical_formula_sum            'B2 O10 Pb4 S'
_chemical_formula_weight         1042.44
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 110.770(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.9363(4)
_cell_length_b                   15.8784(8)
_cell_length_c                   9.6053(5)
_cell_measurement_reflns_used    4303
_cell_measurement_temperature    294.1(3)
_cell_measurement_theta_max      29.8460
_cell_measurement_theta_min      4.0400
_cell_volume                     989.15(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.1(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7908
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.39
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    68.127
_exptl_absorpt_correction_T_max  0.066
_exptl_absorpt_correction_T_min  0.023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    7.000
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       granular
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.975
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.319
_refine_ls_extinction_coef       0.00098(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0171P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0487
_reflns_number_gt                2003
_reflns_number_total             2173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2018-260-39.cif
_cod_data_source_block           Pb4SB2O10
_cod_original_cell_volume        989.15(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1561146