Reinvestigation of the Pb~2~[B~5~O~9~]Br structure based on single-crystal data
Yakubovich, Olga V.; Mochenova, Natalya N.; Dimitrova, Olga. V.; Massa, Werner; Acta Crystallographica, Section E 60 (2004) i127–i130; doi:10.1107/S1600536804023232

data_2204579
_publ_section_title
;
Reinvestigation of the Pb~2~[B~5~O~9~]Br structure based on single-crystal data
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              i127
_journal_page_last               i130
_journal_paper_doi               10.1107/S1600536804023232
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Pb2 (B5 O9) Br]'
_chemical_formula_moiety         'B5 Br O9 Pb2'
_chemical_formula_structural     'Pb2 (B5 O9) Br'
_chemical_formula_sum            'B5 Br O9 Pb2'
_chemical_formula_weight         692.34
_chemical_name_systematic
;
Dilead pentaborate bromide
;
_space_group_IT_number           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_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                   11.4935(19)
_cell_length_b                   11.4717(19)
_cell_length_c                   6.5297(11)
_cell_measurement_reflns_used    4734
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36.0
_cell_measurement_theta_min      3.5
_cell_volume                     860.9(2)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2000)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_database_code_amcsd             0010437
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS-II'
_diffrn_measurement_method       \w
_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  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7497
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         3.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    43.731
_exptl_absorpt_correction_T_max  0.3868
_exptl_absorpt_correction_T_min  0.0933
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(XPREP in SHELXTL; Sheldrick, 1996).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    5.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.022
_refine_diff_density_max         1.955
_refine_diff_density_min         -2.127
_refine_ls_abs_structure_details 'Flack (1983), 1059 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_coef       0.00036(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         2544
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0337P)^2^+13.5461P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0803
_reflns_number_gt                2429
_reflns_number_total             2544
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm6030.cif
_cod_database_code               2204579
_amcsd_formula_title             Pb2[B5O9]Br