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_1569835
_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            'C66 H126 Cu Mo9 N5 O39 P3'
_chemical_formula_weight         2633.62
_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
;
2023-07-18 deposited with the CCDC.	2023-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 105.5757(15)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   27.4763(4)
_cell_length_b                   21.2915(3)
_cell_length_c                   17.3843(3)
_cell_measurement_reflns_used    47230
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      31.1260
_cell_measurement_theta_min      2.2590
_cell_volume                     9796.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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 0.822
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            72602
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.708
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.184
_diffrn_reflns_theta_min         1.868
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5284
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.140
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Flack x determined using 8472 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         22455
_refine_ls_number_restraints     245
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+34.4978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.722
_reflns_Friedel_fraction_full    0.891
_reflns_Friedel_fraction_max     0.594
_reflns_number_gt                21155
_reflns_number_total             22455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03713d2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1569834--1569837.cif.'
_cod_original_cell_volume        9796.6(2)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1569835
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.944
_shelx_res_checksum              11008
_shelx_fab_checksum              31263