Pb4(OH)4(BrO3)3(NO3): An Example of SHG Crystal in Metal Bromates Containing π-Conjugated Planar Triangle.
Kong, Fang; Hu, Chun-Li; Liang, Ming-Li; Mao, Jiang-Gao; Inorganic chemistry 55 (2016) 948–955; doi:10.1021/acs.inorgchem.5b02523

data_4344605
_publ_section_title
;
 Pb4(OH)4(BrO3)3(NO3): An Example of SHG Crystal in Metal Bromates
 Containing \p-Conjugated Planar Triangle.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              948
_journal_page_last               955
_journal_paper_doi               10.1021/acs.inorgchem.5b02523
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'Br3 H4 N O16 Pb4'
_chemical_formula_weight         1342.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.209(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.5988(2)
_cell_length_b                   16.7478(5)
_cell_length_c                   12.8198(4)
_cell_measurement_reflns_used    4415
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.9086
_cell_measurement_theta_min      2.4273
_cell_volume                     1631.13(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3503
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11674
_diffrn_reflns_theta_full        34.32
_diffrn_reflns_theta_max         34.32
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    48.590
_exptl_absorpt_correction_T_max  0.282
_exptl_absorpt_correction_T_min  0.066
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.1079
_exptl_crystal_size_mid          0.0502
_exptl_crystal_size_min          0.0362
_refine_diff_density_max         1.796
_refine_diff_density_min         -1.524
_refine_diff_density_rms         0.322
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(9)
_refine_ls_extinction_coef       0.000080(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   0.975
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         5195
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0553
_reflns_number_gt                4462
_reflns_number_total             5195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02523_si_002.cif
_cod_data_source_block           Pb4H4Br3NO16
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4344605