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_2022196
_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          '(C7 H9 N4 O2)3 [P W12 O40], 1.5C2 H6 O'
_chemical_formula_moiety
'3(C7 H9 N4 O2 +), O40 P W12 3-, 1.5(C2 H6 O)'
_chemical_formula_sum            'C24 H36 N12 O47.5 P W12'
_chemical_formula_weight         3489.82
_chemical_name_common
;
Tris(theobrominium)
\m~12~-phosphato-tetracosa-\m~2~-oxido-dodecaoxidododecatungsten
ethanol sesquisolvate
;
_chemical_name_systematic
;
Tris(3,7-dimethylxanthinium)
\m~12~-phosphato-tetracosa-\m~2~-oxido-dodecaoxidododecatungsten
ethanol sesquisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 90.720(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   23.4412(13)
_cell_length_c                   23.6644(10)
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_cell_measurement_theta_max      26.081
_cell_measurement_theta_min      2.446
_cell_volume                     5994.5(5)
_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      203(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29521
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.081
_diffrn_reflns_theta_min         2.446
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    23.067
_exptl_absorpt_correction_T_max  0.2311
_exptl_absorpt_correction_T_min  0.1939
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_exptl_absorpt_process_details
;
[X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]
;
_exptl_crystal_colour            yellow
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_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
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_refine_ls_number_reflns         11783
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                7160
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jx3058sup1.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C24 H36 N12 O47.50 P W12'
_cod_database_code               2022196
_shelx_estimated_absorpt_t_min   0.076
_shelx_estimated_absorpt_t_max   0.103
_shelx_hkl_checksum              46709
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_cod_database_fobs_code 2022196