Molecular hybrids of trivacant lacunary polyoxomolybdate and multidentate organic ligands.
Jimbo, Atsuhiro; Li, Chifeng; Yonesato, Kentaro; Ushiyama, Tomoki; Yamaguchi, Kazuya; Suzuki, Kosuke; Chemical science 14 (2023) 10280–10284; doi:10.1039/d3sc03713d

data_1569834
_publ_section_title
;
 Molecular hybrids of trivacant lacunary polyoxomolybdate and multidentate
 organic ligands.
;
_journal_issue                   37
_journal_name_full               'Chemical science'
_journal_page_first              10280
_journal_page_last               10284
_journal_paper_doi               10.1039/d3sc03713d
_journal_volume                  14
_journal_year                    2023
_chemical_formula_sum            'C52 H114 Mo9 N3 O34 P'
_chemical_formula_weight         2219.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-07-18 deposited with the CCDC.	2023-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 115.367(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   26.5817(7)
_cell_length_b                   14.4781(2)
_cell_length_c                   24.2574(8)
_cell_measurement_reflns_used    25999
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.3860
_cell_measurement_theta_min      2.0500
_cell_volume                     8435.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0452
_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       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            82798
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.905
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4448
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         6.538
_refine_diff_density_min         -2.052
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         17230
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0798
_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^)+(0.0959P)^2^+166.4525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2020
_refine_ls_wR_factor_ref         0.2115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13992
_reflns_number_total             17230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03713d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 1569834--1569837.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1569834
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              25051
_shelx_fab_checksum              80130