Tetrakis(1,4-dimethylpyridinium) dodecamolybdophosphate nitrate
Xue-Jie Tan; Si-Xiu Sun; Jian-Ping Ma; Shu-Lian Liu; Dian-Xiang Xing; Acta Crystallographica Section E 61 (2005) m711–m713; doi:10.1107/S1600536805008044

data_2205566
_publ_section_title
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 Tetrakis(1,4-dimethylpyridinium) dodecamolybdophosphate nitrate
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_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m711
_journal_page_last               m713
_journal_paper_doi               10.1107/S1600536805008044
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '(C7 H10 N)4 [Mo12 O40 P] N O3'
_chemical_formula_moiety         '4C7 H10 N + , Mo12 O40 P 3- , N O3 -'
_chemical_formula_sum            'C28 H40 Mo12 N5 O43 P'
_chemical_formula_weight         2316.90
_chemical_name_systematic
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Tetrakis(1,4-dimethylpyridinium) dodecamolybdophosphate nitrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 109.679(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.271(6)
_cell_length_b                   11.200(3)
_cell_length_c                   23.316(6)
_cell_measurement_reflns_used    380
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      7.5
_cell_volume                     5968(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (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      291(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16331
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.564
_exptl_absorpt_correction_T_max  0.757
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.579
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             4424
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.466
_refine_diff_density_min         -0.957
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         6338
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0810
_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^)+(0.0788P)^2^+19.95P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1831
_reflns_number_gt                4283
_reflns_number_total             6338
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6490.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 (4 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 (4 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2205566
_cod_database_fobs_code          2205566