Heptabismuthate [Bi7I24]3-: A Main Group Element Anderson-Type Structure and Its Relationships with the Polyoxometalates
Kirill Yu. Monakhov; Christophe Gourlaouen; Roberto Pattacini; Pierre Braunstein; Inorganic Chemistry 51 (2012) 1562–1568; doi:10.1021/ic201859c

data_4328164
_publ_contact_author_address
;Laboratoire de Chimie de Coordination,
 Institut de Chimie (UMR 7177 CNRS), 
Universit\'e de Strasbourg,        
4 rue Blaise Pascal, F-67081 Strasbourg Cedex, France
;
_publ_contact_author_email       braunstein@unistra.fr
_publ_contact_author_fax         '+ 33368851322'
_publ_contact_author_name        'Pierre Braunstein'
_publ_contact_author_phone       +3368851308
_publ_section_title
;
 Heptabismuthate [Bi7I24]3-: A Main Group Element Anderson-Type Structure
 and Its Relationships with the Polyoxometalates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1562
_journal_page_last               1568
_journal_paper_doi               10.1021/ic201859c
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         '3(C20 H38 Bi O8), Bi7 I24, 4(O)'
_chemical_formula_sum            'C60 H114 Bi10 I24 O28'
_chemical_formula_weight         6418.91
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   27.2955(7)
_cell_length_b                   27.2955(7)
_cell_length_c                   31.6049(13)
_cell_measurement_reflns_used    10430
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      0.998
_cell_volume                     20392.3(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            7897
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         3.17
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    18.395
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_correction_T_min  0.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'L. Spek, J. Appl.Cryst. 2003, 36, 7 and 1995, A51, 33'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.136
_exptl_crystal_description       plate
_exptl_crystal_F_000             16800
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.430
_refine_diff_density_min         -3.616
_refine_diff_density_rms         0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         4091
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1088P)^2^+438.2284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.2155
_reflns_number_gt                2395
_reflns_number_total             4091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201859c_si_002.cif
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4328164