Supramolecular networks supported by the anion···π linkage of Keggin-type heteropolyoxotungstates
Panteleieva, Olha S.; Ponomarova, Vira V.; Shtemenko, Alexander V.; Domasevitch, Kostiantyn V.; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S205322962000950X

data_2022195
_publ_section_title
;
 Supramolecular networks supported by the anion&#x00B7;&#x00B7;&#x00B7;\p
 linkage of Keggin-type heteropolyoxotungstates
;
_journal_coeditor_code           JX3058
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205322962000950X
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '(C8 H11 N4 O2)4 [Si W12 O40], 3H2 O'
_chemical_formula_moiety         '4(C8 H11 N4 O2 +), O40 Si W12 4-, 3(H2 O)'
_chemical_formula_sum            'C32 H50 N16 O51 Si W12'
_chemical_formula_weight         3709.17
_chemical_name_common
;
Tetrakis(caffeinium)
\m~12~-silicato-tetracosa-\m~2~-oxido-dodecaoxidododecatungsten
trihydrate
;
_chemical_name_systematic
;
Tetrakis(1,3,7-trimethylxanthinium)
\m~12~-silicato-tetracosa-\m~2~-oxido-dodecaoxidododecatungsten
trihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 107.576(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8623(4)
_cell_length_b                   20.7547(6)
_cell_length_c                   21.8096(6)
_cell_measurement_reflns_used    34632
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.700
_cell_measurement_theta_min      1.666
_cell_volume                     6844.9(3)
_computing_cell_refinement
;
IPDS Software (Stoe & Cie, 2000)
;
_computing_data_collection
;
IPDS Software (Stoe & Cie, 2000)
;
_computing_data_reduction
;
IPDS Software (Stoe & Cie, 2000)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Stoe Image plate diffraction system'
_diffrn_measurement_method       '\f oscillation scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34632
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.700
_diffrn_reflns_theta_min         1.666
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    20.212
_exptl_absorpt_correction_T_max  0.229
_exptl_absorpt_correction_T_min  0.093
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.599
_exptl_crystal_description       prism
_exptl_crystal_F_000             6656
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.349
_refine_diff_density_min         -1.779
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.40(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         9899
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+63.6090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1336
_reflns_number_gt                8741
_reflns_number_total             9899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jx3058sup1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2022195
_shelx_estimated_absorpt_t_min   0.095
_shelx_estimated_absorpt_t_max   0.140
_shelx_hkl_checksum              82897
_shelx_res_checksum              21556
_cod_database_fobs_code 2022195