Tetrapyridinium α-dodecamolybdosilicate hemihydrate
Dang, Dong-Bin; Jin, Ya-Nan; Acta Crystallographica Section E 63 (2007) m881–m883; doi:10.1107/S1600536807007040

data_2212457
_publ_section_title
;
 Tetrapyridinium \a-dodecamolybdosilicate hemihydrate
;
_journal_coeditor_code           BI2142
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m881
_journal_page_last               m883
_journal_paper_doi               10.1107/S1600536807007040
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C5 H6 N)4 [Si Mo12 O40] , 0.5H2 O'
_chemical_formula_moiety         '4C5 H6 N + , Mo12 O40 Si1 4- , 0.5H2 O'
_chemical_formula_sum            'C20 H25 Mo12 N4 O40.5 Si'
_chemical_formula_weight         2148.81
_chemical_name_systematic
;
Tetrapyridinium \a-dodecamolybdosilicate hemihydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.670(3)
_cell_length_b                   20.950(4)
_cell_length_c                   13.996(3)
_cell_measurement_reflns_used    125
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.05
_cell_measurement_theta_min      2.01
_cell_volume                     4887.9(17)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23971
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.106
_exptl_absorpt_correction_T_max  0.537
_exptl_absorpt_correction_T_min  0.479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.920
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4060
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.818
_refine_diff_density_min         -1.568
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         4413
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0542
_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^)+(0.075P)^2^+61.8506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1498
_reflns_number_gt                3984
_reflns_number_total             4413
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi2142.cif
_cod_data_source_block           I
_cod_original_cell_volume        4887.8(17)
_cod_original_formula_sum        'C20 H25 Mo12 N4 O40.50 Si'
_cod_database_code               2212457
_cod_database_fobs_code          2212457