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

data_2108874
_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          '(C5 H14 N3)3 [Bi2 Cl9]'
_chemical_formula_moiety         '3(C5 H14 N3 +), Bi2 Cl9 -'
_chemical_formula_sum            'C15 H42 Bi2 Cl9 N9'
_chemical_formula_weight         1085.59
_chemical_name_systematic
;
Tris(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylguanidinium) 
tri-\m-chlorido-bis[trichloridobismuthate(III)]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 106.6342(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.57031(17)
_cell_length_b                   29.2063(4)
_cell_length_c                   12.04367(19)
_cell_measurement_reflns_used    12505
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      3.04
_cell_volume                     3562.52(10)
_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  0.0230
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23916
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.083
_exptl_absorpt_coefficient_mu    10.563
_exptl_absorpt_correction_T_max  0.27
_exptl_absorpt_correction_T_min  0.21
_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    2.024
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.00220(4)
_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   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6979
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+1.9280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0358
_refine_ls_wR_factor_ref         0.0370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6102
_reflns_number_total             6979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xk5082sup1.cif
_cod_data_source_block           TmgBiCl_3_295K
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2108874
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              31880
_shelx_hkl_checksum              2407
_cod_database_fobs_code 2108874