Supramolecular network of a framework material supported by the anion-π linkage of Keggin-type heteropolyoxotungstates: experimental and theoretical insights.
Samaniyan, Maryam; Mirzaei, Masoud; Gomila, Rosa M.; Eshtiagh-Hosseini, Hossein; Lotfian, Nahid; Mague, Joel T.; Pour, Ali Nakhaei; Frontera, Antonio; Dalton transactions (Cambridge, England : 2003) 50 (2021) 1895–1900; doi:10.1039/d0dt03891a

data_7706423
_publ_section_title
;
 Supramolecular network of a framework material supported by the anion-\p
 linkage of Keggin-type heteropolyoxotungstates: experimental and
 theoretical insights.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1895
_journal_page_last               1900
_journal_paper_doi               10.1039/d0dt03891a
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C21 H33 N3 Na O67 Si Tb3 W12, 10(H2 O), 2(O)'
_chemical_formula_sum            'C21 H53 N3 Na O79 Si Tb3 W12'
_chemical_formula_weight         4345.70
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-09-05 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.080(2)
_cell_length_b                   18.080(2)
_cell_length_c                   20.905(3)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.100
_cell_measurement_theta_min      2.252
_cell_volume                     5918.0(13)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2016)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2016)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2016)'
_computing_molecular_graphics    '<i>DIAMOND</i> (Brandenburg & Putz, 2012)'
_computing_publication_material  '<i>SHELXTL</i> (Bruker, 2016)'
_computing_structure_refinement
'<i>SHELXL-2018/1</i> (Sheldrick, 2015<i>b</i>)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38417
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        29.200
_diffrn_reflns_theta_max         29.249
_diffrn_reflns_theta_min         1.625
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    20.212
_exptl_absorpt_correction_T_max  0.13
_exptl_absorpt_correction_T_min  0.10
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Krause <i>et al.</i>, 2015)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    3.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5820
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.172
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.324
_refine_diff_density_max         3.940
_refine_diff_density_min         -2.669
_refine_diff_density_rms         0.309
_refine_ls_abs_structure_details
;
 Flack x determined using 2943 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons <i>et al.</i>, 2013).
;
_refine_ls_abs_structure_Flack   0.003(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         7090
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0539P)^2^+4.6626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.984
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                6469
_reflns_number_total             7090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03891a2.cif
_cod_data_source_block           jtm1136_0m_a_sq
_cod_depositor_comments          'Adding full bibliography for 7706423.cif.'
_cod_original_cell_volume        5918.3(17)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7706423
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.095
_shelx_estimated_absorpt_t_max   0.129
_shelx_res_checksum              3883
_shelx_fab_checksum              54937