Polyoxometalate-based CuII/CoII complexes tuned using various metal–pyrazole loops: design, diverse architectures and catalytic activity toward the oxidation of thioether derivatives
Zhang, Jing-Yuan; Zhang, Yu-Chen; Wang, Xiu-Li; Chang, Zhi-Han; Zhang, Zhong; Lin, Hong-Yan; Cui, Zi-Wei; CrystEngComm  (2022) –; doi:10.1039/D2CE00074A

data_7244615
_publ_section_title
;
 Polyoxometalate-based CuII/CoII complexes tuned using various
 metal--pyrazole loops: design, diverse architectures and catalytic
 activity toward the oxidation of thioether derivatives
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00074A
_journal_year                    2022
_chemical_formula_moiety
'C56 H80 Cr Cu8 Mo6 N24 O42, 2(Cr Mo6 O24), 4(H2 O)'
_chemical_formula_sum            'C56 H88 Cr3 Cu8 Mo18 N24 O94'
_chemical_formula_weight         4992.74
_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   mixed
_audit_creation_date             2020-12-04
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-03-17 deposited with the CCDC.	2022-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.0760(10)
_cell_angle_beta                 113.7400(10)
_cell_angle_gamma                105.5220(10)
_cell_formula_units_Z            1
_cell_length_a                   15.0645(6)
_cell_length_b                   15.3364(6)
_cell_length_c                   17.7822(7)
_cell_measurement_reflns_used    5647
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     3595.7(2)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      296.15
_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 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f 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  0.0276
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24977
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.437
_diffrn_reflns_theta_min         1.532
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.987
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         16295
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11921
_reflns_number_total             16295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00074a2.cif
_cod_data_source_block           20191219_czh02_0m_sq
_cod_database_code               7244615
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O5W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Free rotating group:
 O5W(H5WA,H5WB), O6W(H6WA,H6WB)
3.b Rotating group:
 O4W(H4WA,H4WB), O2W(H2WA,H2WB), O1W(H1WA,H1WB), O3W(H3WA,H3WB)
3.c Ternary CH refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C18(H18)
3.d Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B)
3.e Aromatic/amide H refined with riding coordinates:
 N9(H9), N10(H10), N11(H11), C5(H5), N12(H12), C6(H6), C7(H7), C8(H8),
 C16(H16), C17(H17), C19(H19), C28(H28)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92643
_shelx_hkl_checksum              24135
_shelx_fab_checksum              18594
_olex2_submission_special_instructions 'No special instructions were received'