Halobismuth(III) salts with substituted aminopyridinium cations
Senior, Levi; Linden, Anthony; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S2053229620006130

data_2022113
_publ_section_title
;
 Halobismuth(III) salts with substituted aminopyridinium cations
;
_journal_coeditor_code           FP3085
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229620006130
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '(C5 H9 N3)2 [Bi Cl6] Cl, H2 O'
_chemical_formula_moiety         '2(C5 H9 N3 1+), Bi Cl6 3-, Cl 1-, H2 O'
_chemical_formula_sum            'C10 H20 Bi Cl7 N6 O'
_chemical_formula_weight         697.45
_chemical_name_systematic
;
Bis(2-amino-3-ammoniopyridinium) hexachloridobismuth(III) chloride monohydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                94.303(4)
_cell_angle_beta                 101.914(4)
_cell_angle_gamma                106.254(4)
_cell_formula_units_Z            2
_cell_length_a                   9.1612(4)
_cell_length_b                   10.8591(6)
_cell_length_c                   11.7273(7)
_cell_measurement_reflns_used    5333
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      29.1560
_cell_measurement_theta_min      3.5200
_cell_volume                     1084.89(11)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009) and Mercury (Macrae <i>et al.</i>,
2020)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b) and PLATON (Spek, 2015,
2020)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      160(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_device       'four-circle \k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova dual radiation'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8459
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.417
_diffrn_reflns_theta_min         2.848
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.001
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2018)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.135
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.534
_refine_diff_density_min         -1.744
_refine_ls_extinction_coef       0.00175(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         5054
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0172P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                4589
_reflns_number_total             5056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fp3085sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_hydrogens' value 'geom & difmap' was
changed to 'mixed'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        1084.89(10)
_cod_database_code               2022113
_shelx_estimated_absorpt_t_min   0.212
_shelx_estimated_absorpt_t_max   0.466
_shelx_hkl_checksum              44683
_shelx_res_checksum              6647
_cod_database_fobs_code 2022113