Tetrakis(1,4-dimethylpyridinium) dodecamolybdosilicate
Xue-Jie Tan; Si-Xiu Sun; Lian-Dong Liu; Jian-Ping Ma; Dian-Xiang Xing; Acta Crystallographica Section E 61 (2005) m1620–m1622; doi:10.1107/S1600536805023111

data_2206598
_publ_section_title
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 Tetrakis(1,4-dimethylpyridinium) dodecamolybdosilicate
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_journal_coeditor_code           XU6013
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1620
_journal_page_last               m1622
_journal_paper_doi               10.1107/S1600536805023111
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '(C7 H10 N)4 [Si Mo12 O40]'
_chemical_formula_moiety         '4C7 H10 N +, Mo12 O40 Si 4-'
_chemical_formula_sum            'C28 H40 Mo12 N4 O40 Si'
_chemical_formula_weight         2252.01
_chemical_name_systematic
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Tetrakis(1,4-dimethylpyridinium) dodecamolybdosilicate
;
_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                69.081(5)
_cell_angle_beta                 77.369(4)
_cell_angle_gamma                66.626(5)
_cell_formula_units_Z            1
_cell_length_a                   11.033(5)
_cell_length_b                   11.951(5)
_cell_length_c                   12.034(5)
_cell_measurement_reflns_used    378
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.82
_cell_volume                     1355.0(10)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.94
_diffrn_measured_fraction_theta_max 0.94
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8908
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.8
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.807
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1074.0
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.494
_refine_diff_density_min         -1.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         4474
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.101
_refine_ls_R_factor_gt           0.100
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+102.4837P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.225
_refine_ls_wR_factor_ref         0.226
_reflns_number_gt                4355
_reflns_number_total             4474
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu6013.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (20 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (20 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_original_cell_volume        1355.1(10)
_cod_database_code               2206598
_cod_database_fobs_code          2206598