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_1571651
_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_moiety
'C36 H30 Mo18 N12 O62 P2, 3(C16 H36 N), 4(C2 H4 Cl2)'
_chemical_formula_sum            'C92 H154 Cl8 Mo18 N15 O62 P2'
_chemical_formula_weight         4534.75
_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   geom
_audit_creation_date             2024-02-20
_audit_creation_method           'Olex2 1.5'
_audit_update_record
;
2024-04-03 deposited with the CCDC.	2024-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6111(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.1448(3)
_cell_length_b                   27.3825(3)
_cell_length_c                   29.9056(5)
_cell_measurement_reflns_used    36664
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      14.9900
_cell_measurement_theta_min      0.6970
_cell_volume                     21848.5(5)
_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_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'PILATUS3 X CdTe 1M'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      0.00 180.00   0.50    1.00    --    0.00  45.00   0.00  360
  2  \w      0.00 180.00   0.50    1.00    --    0.00  45.00 -90.00  360
;
_diffrn_measurement_device       'SPring-8 BL02B1'
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0110553000
_diffrn_orient_matrix_UB_12      -0.0044720000
_diffrn_orient_matrix_UB_13      0.0069895000
_diffrn_orient_matrix_UB_21      0.0010397000
_diffrn_orient_matrix_UB_22      0.0132354000
_diffrn_orient_matrix_UB_23      0.0068176000
_diffrn_orient_matrix_UB_31      -0.0108535000
_diffrn_orient_matrix_UB_32      0.0058030000
_diffrn_orient_matrix_UB_33      -0.0101497000
_diffrn_radiation_monochromator  Si(311)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4142
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            302178
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        14.390
_diffrn_reflns_theta_max         15.003
_diffrn_reflns_theta_min         0.653
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79018
_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            colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8916
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.121
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1933
_refine_ls_number_reflns         44637
_refine_ls_number_restraints     741
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0645
_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^)+(0.1011P)^2^+58.3815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31641
_reflns_number_total             44637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02384f2.cif
_cod_data_source_block           Compound_II
_cod_depositor_comments
'Adding full bibliography for 1571650--1571653.cif.'
_cod_database_code               1571651
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.928
_shelx_res_checksum              59275
_shelx_fab_checksum              10240
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.278
_oxdiff_exptl_absorpt_empirical_full_min 0.845