Crystal structure of tris(4-aminopyridinium)phosphato-polyoxo-dodecamolybdate — 4-aminopyridine — water (1:1:1), [C5H7N2]3[PMo12O40] · C5H6N2 · H2O
Xiang-Jiang Wu; Shu-Zi Lü; Qing Cai; Chuan-Lei Zhang; Tie-Jun Cai; Zeitschrift für Kristallographie - New Crystal Structures 226 (2011) 389–; doi:

data_8103146
_publ_section_title
;
 Crystal structure of
 tris(4-aminopyridinium)phosphato-polyoxo-dodecamolybdate ---
 4-aminopyridine --- water (1:1:1), [C5H7N2]3[PMo12O40] &#x00B7; C5H6N2
 &#x00B7; H2O
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              389
_journal_volume                  226
_journal_year                    2011
_chemical_formula_sum            'C20 H29 Mo12 N8 O41 P'
_chemical_formula_weight         2219.76
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.2050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7094(4)
_cell_length_b                   25.7946(9)
_cell_length_c                   16.6748(6)
_cell_measurement_reflns_used    4276
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      1.58
_cell_volume                     4996.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15366
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.054
_exptl_absorpt_correction_T_max  0.5157
_exptl_absorpt_correction_T_min  0.4416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.951
_exptl_crystal_density_meas      2.948
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4208
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.298
_refine_diff_density_min         -2.606
_refine_diff_density_rms         0.239
_refine_ls_extinction_coef       0.00112(7)
_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   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4276
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0921P)^2^+105.4530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                3903
_reflns_number_total             4276
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3402.cff
_cod_data_source_block           14
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               8103146