Crystal structure of tetrakispyridinium hexakis(m3-oxo)-hexakis(m2-oxo)tetradecaoxo-octamolybdenum, [C5H6N]4[Mo8O26]
Hai-Xing Liu; Zeitschrift für Kristallographie - New Crystal Structures 225 (2010) 91–; doi:

data_8102609
_publ_section_title
;
 Crystal structure of tetrakispyridinium
 hexakis(m3-oxo)-hexakis(m2-oxo)tetradecaoxo-octamolybdenum,
 [C5H6N]4[Mo8O26]
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              91
_journal_volume                  225
_journal_year                    2010
_chemical_formula_sum            'C10 H12 Bi0 Mo4 N2 O13'
_chemical_formula_weight         751.98
_chemical_name_systematic
; 
tetrakispyridinium hexakis(m3-oxo)-
hexakis(m2-oxo)tetradecaoxo-octamolybdenum 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.815(8)
_cell_angle_beta                 76.494(9)
_cell_angle_gamma                69.154(8)
_cell_formula_units_Z            2
_cell_length_a                   9.599(6)
_cell_length_b                   9.993(6)
_cell_length_c                   10.699(6)
_cell_measurement_reflns_used    2067
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      1.96
_cell_volume                     932.2(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4940
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    2.700
_exptl_absorpt_correction_T_max  0.421
_exptl_absorpt_correction_T_min  0.300
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.288
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3260
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                2387
_reflns_number_total             3260
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2839.cff
_cod_data_source_block           1
_cod_original_cell_volume        932.2(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8102609