Polyoxometalates with separate lacuna sites.
Wang, Wenyan; Izarova, Natalya V.; van Leusen, Jan; Kögerler, Paul; Chemical communications (Cambridge, England) 56 (2020) 14857–14860; doi:10.1039/d0cc05791f

data_7127468
_publ_section_title
;
 Polyoxometalates with separate lacuna sites.
;
_journal_issue                   94
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14857
_journal_page_last               14860
_journal_paper_doi               10.1039/d0cc05791f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_sum            'C24 H128 Cs7.5 K0.5 O178 P8 W32 Y4'
_chemical_formula_weight         10768.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-11-02 deposited with the CCDC.	2020-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                73.56(3)
_cell_angle_beta                 86.69(3)
_cell_angle_gamma                79.61(3)
_cell_formula_units_Z            1
_cell_length_a                   12.902(3)
_cell_length_b                   14.649(3)
_cell_length_c                   24.956(5)
_cell_measurement_reflns_used    5323
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.95
_cell_measurement_theta_min      1.60
_cell_volume                     4449.6(18)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.131.0 (STOE, 2017)
;
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area X-Red32 1.63.2.0 (STOE, 2017) 
;
_computing_molecular_graphics    'Diamond Version 3.2k'
_computing_publication_material  'Diamond Version 3.2k'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1635
_diffrn_reflns_av_unetI/netI     0.1250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            90921
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.317
_diffrn_source                   'Genix Mo'
_exptl_absorpt_coefficient_mu    23.592
_exptl_absorpt_correction_T_max  0.4149
_exptl_absorpt_correction_T_min  0.0898
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration.
Afterwards scaling of reflection intensities was performed 
within STOE LANA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.019
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4762
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.123
_refine_diff_density_min         -3.355
_refine_diff_density_rms         0.583
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         15715
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.0815
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1093P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1959
_refine_ls_wR_factor_ref         0.2201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8347
_reflns_number_total             15715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05791f2.cif
_cod_data_source_block           y_a_sq
_cod_original_cell_volume        4449.3(17)
_cod_original_formula_sum        'C24 H128 Cs7.50 K0.50 O178 P8 W32 Y4'
_cod_database_code               7127468
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.088
_shelx_estimated_absorpt_t_max   0.538
_shelx_res_checksum              74895
_shelx_fab_checksum              1279