Crystal structure of (C~9~H~17~N~2~)~3~[Bi~2~I~9~]
James, Zoe; Cai, Yunhe; Vaqueiro, Paz; Acta Crystallographica Section E 77 (2021) –; doi:10.1107/S2056989021007799

data_2243887
_publ_section_title
;
 Crystal structure of (C~9~H~17~N~2~)~3~[Bi~2~I~9~]
;
_journal_coeditor_code           JQ2007
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989021007799
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '(C9 H17 N2)3 [Bi2 I9]'
_chemical_formula_moiety         '3(C9 H17 N2 +), Bi2 I9 3-'
_chemical_formula_sum            'C27 H51 Bi2 I9 N6'
_chemical_formula_weight         2019.79
_chemical_name_systematic
;
Tris(2,3,4,6,7,8,9,10-octahydropyrimido[1,2-<i>a</i>]azepin-1-ium)
tri-\m~2~-iodido-bis[triiodidobismuth(III)]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 115.861(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2590(9)
_cell_length_b                   12.5734(3)
_cell_length_c                   21.6767(9)
_cell_measurement_reflns_used    25746
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33
_cell_measurement_theta_min      2
_cell_volume                     4723.4(4)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
ATOMS (Dowty, 2020) and ORIGIN (Edwards, 2002)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            38319
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         2.350
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.349
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.840
_exptl_crystal_description       plate
_exptl_crystal_F_000             3592
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.070
_refine_diff_density_max         2.221
_refine_diff_density_min         -2.568
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         13780
_refine_ls_number_restraints     543
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0423P)^2^+1.9329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                11096
_reflns_number_total             13780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jq2007sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2243887
_shelx_estimated_absorpt_t_min   0.104
_shelx_estimated_absorpt_t_max   0.455
_shelx_hkl_checksum              59378
_shelx_res_checksum              32609
_cod_database_fobs_code 2243887