Pb2B3O5.5(OH)2 and [Pb3(B3O7)](NO3): Facile Syntheses of New Lead(II) Borates by Simply Changing the pH Values of the Reaction Systems
Jun-Ling Song; Chun-Li Hu; Xiang Xu; Fang Kong; Jiang-Gao Mao; Inorganic Chemistry 52 (2013) 8979–8986; doi:10.1021/ic401175r

data_4335617
_publ_section_title
;
 Pb2B3O5.5(OH)2 and [Pb3(B3O7)](NO3): Facile Syntheses of New Lead(II)
 Borates by Simply Changing the pH Values of the Reaction Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8979
_journal_page_last               8986
_journal_paper_doi               10.1021/ic401175r
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'B3 H2 O7.5 Pb2'
_chemical_formula_weight         568.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           34
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5824(7)
_cell_length_b                   11.7664(7)
_cell_length_c                   4.5657(2)
_cell_measurement_reflns_used    2920
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2391
_cell_measurement_theta_min      3.4563
_cell_volume                     622.23(6)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3503
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            4064
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         3.46
_diffrn_standards_number         2916
_exptl_absorpt_coefficient_mu    54.041
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19012
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    6.072
_exptl_crystal_description       needle
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.2500
_exptl_crystal_size_mid          0.0300
_exptl_crystal_size_min          0.0200
_refine_diff_density_max         0.814
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(18)
_refine_ls_extinction_coef       0.00126(9)
_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   0.994
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1237
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0093P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0385
_refine_ls_wR_factor_ref         0.0394
_reflns_number_gt                1146
_reflns_number_total             1237
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401175r_si_001_2.cif
_cod_data_source_block           Pb2B3O7.5H2
_cod_original_formula_sum        'B3 H2 O7.50 Pb2'
_cod_database_code               4335617