Tris(pyrrolidin-1-yl)carbenium tri-μ-iodido-bis[triiodidobismuthate(III)]
Tiritiris, Ioannis; Knobloch, Georg; Saur, Stefan; Kantlehner, Willi; IUCrData 1 (2016) x160427–; doi:10.1107/S2414314616004272

data_1542933
_publ_section_title
;
 Tris(pyrrolidin-1-yl)carbenium
 tri-\m-iodido-bis[triiodidobismuthate(III)]
;
_journal_coeditor_code           ZL4007
_journal_issue                   3
_journal_name_full               IUCrData
_journal_page_first              x160427
_journal_paper_doi               10.1107/S2414314616004272
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          '(C13 H24 N3)3 [Bi2 I9]'
_chemical_formula_moiety         '3(C13 H24 N3 +), Bi2 I9 3-'
_chemical_formula_sum            'C39 H72 Bi2 I9 N9'
_chemical_formula_weight         2227.11
_chemical_name_systematic
;
Tris(pyrrolidin-1-yl)carbenium tri-\m-iodido-bis[triiodidobismuthate(III)]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.601(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1643(7)
_cell_length_b                   16.7047(8)
_cell_length_c                   24.9505(12)
_cell_measurement_reflns_used    61942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.538
_cell_measurement_theta_min      1.633
_cell_volume                     5901.2(5)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO'
_diffrn_measurement_method       '\f scans, and \w scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            61942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.538
_diffrn_reflns_theta_min         1.633
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.699
_exptl_absorpt_correction_T_max  0.2755
_exptl_absorpt_correction_T_min  0.0859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.956
_refine_ls_extinction_coef       0.000096(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         9039
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0068P)^2^+14.6985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0330
_refine_ls_wR_factor_ref         0.0339
_reflns_number_gt                8198
_reflns_number_total             9039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zl4007sup1.cif
_cod_data_source_block           I
_cod_database_code               1542933
_shelx_hkl_checksum              67680
_shelx_res_checksum              14126
_cod_database_fobs_code 1542933