Self-assembled molecular hybrids comprising lacunary polyoxometalates and multidentate imidazole ligands.
Sun, Haoran; Jimbo, Atsuhiro; Li, Chifeng; Yonesato, Kentaro; Yamaguchi, Kazuya; Suzuki, Kosuke; Chemical science 15 (2024) 9281–9286; doi:10.1039/d4sc02384f

data_1571652
_publ_section_title
;
 Self-assembled molecular hybrids comprising lacunary polyoxometalates and
 multidentate imidazole ligands.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              9281
_journal_page_last               9286
_journal_paper_doi               10.1039/d4sc02384f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C60 H48 Mo36 N24 O124 P4'
_chemical_formula_weight         6666.94
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-04-03 deposited with the CCDC.	2024-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.2789(3)
_cell_length_b                   39.2789(3)
_cell_length_c                   32.7662(5)
_cell_measurement_reflns_used    30218
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      13.7580
_cell_measurement_theta_min      0.7620
_cell_volume                     50552.7(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'RAPID AUTO (Rigaku OD)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'PILATUS3 X CdTe 1M'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'SPring-8 BL02B1'
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4151
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            275758
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        13.965
_diffrn_reflns_theta_max         13.965
_diffrn_reflns_theta_min         0.606
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.876
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12560
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         20837
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1102P)^2^+78.0267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12405
_reflns_number_total             20837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02384f2.cif
_cod_data_source_block           Compound_IV
_cod_depositor_comments
'Adding full bibliography for 1571650--1571653.cif.'
_cod_original_cell_volume        50552.7(11)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1571652
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.925
_shelx_estimated_absorpt_t_max   0.949
_oxdiff_exptl_absorpt_empirical_full_min 0.574
_oxdiff_exptl_absorpt_empirical_full_max 2.142
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_shelx_res_checksum              97819
_shelx_fab_checksum              51600