Polyoxomolybdate-Supported Bismuth Trihalides [Mo8O26(BiX3)2](4-) (X = Cl, Br, I): Syntheses and Study of Polymorphism.
Adonin, Sergey A.; Peresypkina, Eugenia V.; Sokolov, Maxim N.; Korolkov, Ilya V.; Fedin, Vladimir P.; Inorganic chemistry 53 (2014) 6886–6892; doi:10.1021/ic500710t

data_4340006
_publ_section_title
;
 Polyoxomolybdate-Supported Bismuth Trihalides [Mo8O26(BiX3)2](4-) (X =
 Cl, Br, I): Syntheses and Study of Polymorphism.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6886
_journal_page_last               6892
_journal_paper_doi               10.1021/ic500710t
_journal_volume                  53
_journal_year                    2014
_chemical_formula_structural     '(TBA)4 [Mo8 O26 (Bi I3)2]'
_chemical_formula_sum            'C64 H144 Bi2 I6 Mo8 N4 O26'
_chemical_formula_weight         3332.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.1720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.3860(3)
_cell_length_b                   17.3957(2)
_cell_length_c                   17.0461(2)
_cell_measurement_reflns_used    12507
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      34.4764
_cell_measurement_theta_min      3.3398
_cell_volume                     5155.43(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 15.9702
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Mova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33989
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         34.56
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    6.197
_exptl_absorpt_correction_T_max  .762
_exptl_absorpt_correction_T_min  .399
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.2253
_exptl_crystal_size_mid          0.0964
_exptl_crystal_size_min          0.0461
_refine_diff_density_max         1.483
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.778
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         20251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.778
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0486
_reflns_number_gt                11975
_reflns_number_total             20251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500710t_si_001.cif
_cod_data_source_block           compound_3b
_cod_depositor_comments
'Adding full bibliography for 4340001--4340007.cif.'
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               4340006