12-Tungstophosphoric acid‒1,1'-methylenebis(imidazolidine-2,4-dione)‒imidazolidine-2,4-dione‒water (2/1/4/21.5)
Alizadeh, Mohammad Hasan; Mohammadi Zonoz, Irandokht; Acta Crystallographica Section E 66 (2010) m839–; doi:10.1107/S160053681002310X

data_2226573
_publ_section_title
;
 12-Tungstophosphoric
 acid--1,1'-methylenebis(imidazolidine-2,4-dione)--imidazolidine-2,4-dione--water
 (2/1/4/21.5)
;
_journal_coeditor_code           LH5037
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m839
_journal_paper_doi               10.1107/S160053681002310X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'2{H3 [P W12 O40]}, 4C3 H4 N2 O2, C7 H8 N4 O4, 21.5H2 O'
_chemical_formula_moiety
'2(H3 O40 P W12), 4(C3 H4 N2 O2), C7 H8 N4 O4,  21.5(H2 O)'
_chemical_formula_sum            'C19 H73 N12 O113.5 P2 W24'
_chemical_formula_weight         6760.23
_chemical_name_systematic
;
12-Tungstophosphoric
acid--1,1'-methylenebis(imidazolidine-2,4-dione)--imidazolidine-2,4-dione--water
(2/1/4/21.5)
;
_space_group_IT_number           1
_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                71.3280(10)
_cell_angle_beta                 81.3160(10)
_cell_angle_gamma                64.7510(10)
_cell_formula_units_Z            1
_cell_length_a                   12.7271(6)
_cell_length_b                   13.3286(7)
_cell_length_c                   18.9177(9)
_cell_measurement_reflns_used    5550
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.3
_cell_volume                     2749.3(2)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \w 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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0707
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            51543
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    25.148
_exptl_absorpt_correction_T_max  0.215
_exptl_absorpt_correction_T_min  0.031
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2985
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.442
_refine_diff_density_min         -1.321
_refine_ls_abs_structure_details 'Flack (1983), 12649 Friedel pairs'
_refine_ls_abs_structure_Flack   0.492(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1577
_refine_ls_number_reflns         25728
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                22772
_reflns_number_total             25728
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5037.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C19 H73 N12 O113.50 P2 W24'
_cod_database_code               2226573
_cod_database_fobs_code          2226573