Tetrakis(<i>N</i>-ethyl-9-oxo-4-azonia-5-aza-9<i>H</i>-fluorene) tetra-μ~3~-iodo-hexa-μ~2~-iodo-dodecaiodohexabismuthate
Tershansy, Meredith A.; Goforth, Andrea M.; Smith, Mark D.; Peterson Jr, LeRoy; Loye, Hans-Conrad zur; Acta Crystallographica Section E 62 (2006) m3269–m3271; doi:10.1107/S1600536806043960

data_2211567
_publ_section_title
;
 Tetrakis(<i>N</i>-ethyl-9-oxo-4-azonia-5-aza-9<i>H</i>-fluorene)
 tetra-\m~3~-iodo-hexa-\m~2~-iodo-dodecaiodohexabismuthate
;
_journal_coeditor_code           OM2062
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3269
_journal_page_last               m3271
_journal_paper_doi               10.1107/S1600536806043960
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C13 H11 N2 O)4 [Bi6 I22]'
_chemical_formula_moiety         '4C13 H11 N2 O +, Bi6 I22 4-'
_chemical_formula_sum            'C52 H44 Bi6 I22 N8 O4'
_chemical_formula_weight         4890.63
_chemical_name_systematic
;
Tetrakis(<i>N</i>-ethyl-9-oxo-4-azonia-5-aza-9H-fluorene)
tetra-\m~3~-iodo-hexa-\m~2~-iodo-dodecaiodohexabismuthate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 92.5890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3944(10)
_cell_length_b                   17.0764(12)
_cell_length_c                   40.710(3)
_cell_measurement_reflns_used    5414
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      26.376
_cell_measurement_theta_min      2.209
_cell_volume                     9302.0(12)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            48604
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.653
_exptl_absorpt_correction_T_max  0.474
_exptl_absorpt_correction_T_min  0.180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             8432
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.915
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         9574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+84.5173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                8178
_reflns_number_total             9574
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2062.cif
_cod_data_source_block           I
_cod_original_cell_volume        9302.1(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2211567
_cod_database_fobs_code          2211567