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_4340001
_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_moiety         'Bi2 Cl6 Mo8 O26, 4(C16 H36 N), 2(C2 H3 N)'
_chemical_formula_sum            'C68 H150 Bi2 Cl6 Mo8 N6 O26'
_chemical_formula_weight         2866.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.184(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.1078(3)
_cell_length_b                   16.8850(3)
_cell_length_c                   19.3604(3)
_cell_measurement_reflns_used    14847
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      73.6830
_cell_measurement_theta_min      3.8250
_cell_volume                     5147.04(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22877
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         73.87
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    16.242
_exptl_absorpt_correction_T_max  0.331
_exptl_absorpt_correction_T_min  0.063
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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            colourless
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.3274
_exptl_crystal_size_mid          0.2200
_exptl_crystal_size_min          0.0953
_refine_diff_density_max         1.022
_refine_diff_density_min         -2.129
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.000290(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         10020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+3.4285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                8998
_reflns_number_total             10020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500710t_si_001.cif
_cod_data_source_block           compound_1*2MeCN
_cod_depositor_comments
'Adding full bibliography for 4340001--4340007.cif.'
_cod_original_cell_volume        5147.03(15)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4340001
_chemical_melting_structural     '(Bu4 N)4 [Mo8 O26 (Bi Cl3)2] * 2(C2 H3 N)'