Understanding distortions of inorganic substructures in chloridobismuthates(III)
Bujak, Maciej; Acta Crystallographica Section B 77 (2021) –; doi:10.1107/S2052520621004753

data_2108873
_publ_section_title
;
 Understanding distortions of inorganic substructures in
 chloridobismuthates(III)
;
_journal_coeditor_code           XK5082SUP1
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520621004753
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '(C4 H14 N2) [Bi Cl5]'
_chemical_formula_moiety         'C4 H14 N2 2+, Bi Cl5 2-'
_chemical_formula_sum            'C4 H14 Bi Cl5 N2'
_chemical_formula_weight         476.40
_chemical_name_systematic
;
<i>catena</i>-Poly[<i>N</i>,<i>N</i>-dimethylethane-1,2-diammonium 
[[tetrachloridobismuthate(III)]-\m-chlorido]]
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.60312(9)
_cell_length_b                   12.50404(14)
_cell_length_c                   13.63023(15)
_cell_measurement_reflns_used    8285
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.65
_cell_measurement_theta_min      3.06
_cell_volume                     1295.82(3)
_computing_cell_refinement
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_collection
'CrysAlisCCD 1.171.29.10 (Oxford Diffraction, 2006)'
_computing_data_reduction
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0121
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8742
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_min         3.068
_exptl_absorpt_coefficient_mu    14.596
_exptl_absorpt_correction_T_max  0.22
_exptl_absorpt_correction_T_min  0.06
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 1035 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.031(2)
_refine_ls_extinction_coef       0.00133(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0104
_refine_ls_R_factor_gt           0.0100
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0097P)^2^+0.4838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0236
_refine_ls_wR_factor_ref         0.0237
_reflns_Friedel_coverage         0.718
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2514
_reflns_number_total             2545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xk5082sup1.cif
_cod_data_source_block           NNBiCl_2_295K
_cod_database_code               2108873
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              37253
_shelx_hkl_checksum              21324
_cod_database_fobs_code 2108873