A protecting group strategy to access stable lacunary polyoxomolybdates for introducing multinuclear metal clusters
Li, Chifeng; Jimbo, Atsuhiro; Yamaguchi, Kazuya; Suzuki, Kosuke; Chemical Science 12 (2021) 1240–1244; doi:10.1039/D0SC06133F

data_1560084
_publ_section_title
;
 A protecting group strategy to access stable lacunary polyoxomolybdates
 for introducing multinuclear metal clusters
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1240
_journal_page_last               1244
_journal_paper_doi               10.1039/D0SC06133F
_journal_volume                  12
_journal_year                    2021
_chemical_formula_sum            'C174 H174 Cl20 Mn6 Mo18 O74 P8'
_chemical_formula_weight         6462.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2020-11-01 deposited with the CCDC.	2020-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                95.310(2)
_cell_angle_beta                 112.975(2)
_cell_angle_gamma                99.330(2)
_cell_formula_units_Z            1
_cell_length_a                   17.3006(4)
_cell_length_b                   19.3900(4)
_cell_length_c                   20.7716(4)
_cell_measurement_reflns_used    36246
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.1650
_cell_measurement_theta_min      2.3340
_cell_volume                     6236.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            86736
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         1.507
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.499
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.549
_refine_diff_density_min         -3.345
_refine_diff_density_rms         0.275
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1351
_refine_ls_number_reflns         34193
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0940P)^2^+27.3530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24795
_reflns_number_total             34193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06133f2.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 1560083--1560084.cif.'
_cod_original_cell_volume        6236.6(2)
_cod_database_code               1560084
_oxdiff_exptl_absorpt_empirical_full_min 0.448
_oxdiff_exptl_absorpt_empirical_full_max 1.958
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_shelxl_version_number           2014/6
_shelx_res_checksum              75092
_shelx_fab_checksum              22719