Self-assembly of a novel multicomponent polyoxometalate-based tetrahedral supercluster with high catalytic activity for thioether oxidation
Liu, Xiaodong; Xu, Na; Liu, Xiaohui; Guo, Yanyan; Wang, Xiuli; Chemical Communications  (2022) –; doi:10.1039/D2CC02748H

data_7130834
_publ_section_title
;
 Self-assembly of a novel multicomponent polyoxometalate-based tetrahedral
 supercluster with high catalytic activity for thioether oxidation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02748H
_journal_year                    2022
_chemical_formula_moiety         'Co12 Mo80 O360 P36 Pb4, 12(C7 H7 N2)'
_chemical_formula_sum            'C84 H342 Co12 Mo80 N24 O489 P36 Pb4'
_chemical_formula_weight         19839.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-26
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-09-27 deposited with the CCDC.	2022-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.355(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.9076(13)
_cell_length_b                   57.925(2)
_cell_length_c                   32.2149(16)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      2.36
_cell_volume                     54415(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       69
_diffrn_reflns_limit_k_min       -69
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            292167
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.117
_diffrn_reflns_theta_max         25.117
_diffrn_reflns_theta_min         2.233
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.9
_diffrn_source_power             0.0405
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.587
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             37912
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.615
_refine_diff_density_min         -1.982
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2663
_refine_ls_number_reflns         48305
_refine_ls_number_restraints     714
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+1065.3273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                37338
_reflns_number_total             48305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02748h2.cif
_cod_data_source_block           1
_cod_original_cell_volume        54416(4)
_cod_database_code               7130834
_shelx_shelxl_version_number     2019/2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18
\\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26
\\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34
\\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim
C42: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
3.8A
N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8 \\sim N9
\\sim N10 \\sim N11 \\sim N12: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3.8A
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), N1(H1A), C2(H2), C3(H3), N2(H2A), C4(H4), N3(H3A), N4(H4A), C7(H7),
 C8(H8), C10(H10), C11(H11), C13(H13), N5(H5), N6(H6), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), N7(H7A), C24(H24), C25(H25),
 N8(H8A), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), N9(H9),
 N10(H10A), C36(H36), C37(H37), C38(H38), C39(H39), N11(H11A), N12(H12A),
 C42(H42), C12(H12)
3.b Fitted pentagon refined as free rotating group:
 N3(C5,C6,N4,C7), N9(C34,C35,N10,C36), N11(C40,C41,N12,C42)
3.c Fitted hexagon refined as free rotating group:
 C16(C17,C18,C19,C20,C21)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 5152 electrons were 
found in a volume of 22328\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
126[H2O], 3[H2O] per Asymmetric Unit 
which account for 5160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27670
_shelx_hkl_checksum              7797
_shelx_fab_checksum              54119
_olex2_submission_special_instructions 'No special instructions were received'