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_1569836
_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            'C65 H123 Mo9 N4 O37 P3'
_chemical_formula_weight         2509.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-07-19 deposited with the CCDC.	2023-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 105.7192(18)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   27.5817(4)
_cell_length_b                   21.2628(3)
_cell_length_c                   17.2310(3)
_cell_measurement_reflns_used    49006
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.4950
_cell_measurement_theta_min      1.9270
_cell_volume                     9727.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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      93(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_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  0.0479
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            98347
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.916
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86263
_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            'Pale Yellow'
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5040
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.087
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Flack x determined using 9565 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         28019
_refine_ls_number_restraints     364
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+20.9061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     0.888
_reflns_number_gt                24249
_reflns_number_total             28019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03713d2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
'Adding full bibliography for 1569834--1569837.cif.'
_cod_original_cell_volume        9727.5(3)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1569836
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              49557
_shelx_fab_checksum              75007