Redetermination of K~4~[Bi~2~Cl~10~]·4H~2~O
Khelifi, Mabrouk; Zouari, Ridha; Ben Salah, Abdelhamid; Acta Crystallographica Section E 64 (2008) i80–; doi:10.1107/S1600536808035435

data_2220381
_publ_section_title
;
 Redetermination of K~4~[Bi~2~Cl~10~]&#x00B7;4H~2~O
;
_journal_coeditor_code           WM2201
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i80
_journal_paper_doi               10.1107/S1600536808035435
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'K4 [Bi2 Cl10], 4H2 O'
_chemical_formula_structural     'K4 [Bi2 Cl10] (H2 O)4'
_chemical_formula_sum            'Bi2 Cl10 H8 K4 O4'
_chemical_formula_weight         1000.94
_chemical_name_systematic
;
tetrapotassium di-\m-chlorido-bis[tetrachloridomuthate(III)] tetrahydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.43100(10)
_cell_length_b                   21.8444(3)
_cell_length_c                   12.2561(2)
_cell_measurement_reflns_used    4596
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      34.159
_cell_measurement_theta_min      1.905
_cell_volume                     2257.21(6)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'APEX2 (Bruker, 2006)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2001)
;
_computing_publication_material
'CRYSTALS (Betteridge <i>et al.</i>,  2003) and publCif (Westrip, 2008)'
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008) and CRYSTALS (Betteridge <i>et al.</i>,
2003)
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26961
_diffrn_reflns_theta_full        32.791
_diffrn_reflns_theta_max         34.157
_diffrn_reflns_theta_min         1.905
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.493
_exptl_absorpt_correction_T_max  0.2470
_exptl_absorpt_correction_T_min  0.0670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.945
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.01
_refine_diff_density_min         -0.82
_refine_ls_extinction_coef       33.8(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0831
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2801
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0165
_refine_ls_shift/su_max          0.00188
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.260 0.753E-01 0.968E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0325
_refine_ls_wR_factor_gt          0.0170
_refine_ls_wR_factor_ref         0.0170
_reflns_number_gt                2801
_reflns_number_total             4596
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            wm2201.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P n m a '
_cod_database_code               2220381
_cod_database_fobs_code          2220381