New pyrimidine-amide-tetrazole ligand derived polyoxometalate-based copper complexes as catalysts for sulfide-sulfoxide transformation and electrochemical sensors
Lu, Jun-Jun; Lin, Hong-Yan; Liu, Qian-Qian; Liu, Xiao-Dong; Wang, Xiu-Li; CrystEngComm 25 (2023) 3025–3032; doi:10.1039/D3CE00269A

data_7246657
_publ_section_title
;
 New pyrimidine-amide-tetrazole ligand derived polyoxometalate-based
 copper complexes as catalysts for sulfide-sulfoxide transformation and
 electrochemical sensors
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              3025
_journal_page_last               3032
_journal_paper_doi               10.1039/D3CE00269A
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C12 H18 Cr Cu4 Mo6 N14 O30, 2(H2 O)'
_chemical_formula_sum            'C12 H22 Cr Cu4 Mo6 N14 O32'
_chemical_formula_weight         1756.23
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-05
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-06 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                87.805(2)
_cell_angle_beta                 78.1090(10)
_cell_angle_gamma                73.8390(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8674(7)
_cell_length_b                   13.4431(8)
_cell_length_c                   17.3938(11)
_cell_measurement_reflns_used    1837
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      2.29
_cell_volume                     2387.8(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0454
_diffrn_reflns_av_unetI/netI     0.1000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15660
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.496
_diffrn_reflns_theta_min         1.197
_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    3.582
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         9881
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0270P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5985
_reflns_number_total             9881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00269a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7246657--7246658.cif.'
_cod_database_code               7246657
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H3WB-H5WA_$1
 2.4 with sigma of 0.02
 H4WA-H22
 2.2 with sigma of 0.02
 H5WA-H14
 2.2 with sigma of 0.02
 H5WB-H14
 2.2 with sigma of 0.02
 H4WB-H22
 2.2 with sigma of 0.02
 Cu3-H2WA \\sim Cu3-H2WB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N10) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N6) \\sim Ueq, Uanis(N10) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C12) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.04
Uanis(N7) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C10) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4.a Free rotating group:
 O2W(H2WA,H2WB), O5W(H5WA,H5WB), O4W(H4WA,H4WB)
4.b Rotating group:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB)
4.c Ternary CH refined with riding coordinates:
 O27(H27), O16(H16), O22(H22), O26(H26), O14(H14), O25(H25)
4.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C11(H11), C6(H6), C5(H5), C12(H12), C9(H9)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              88999
_shelx_hkl_checksum              58770
_shelx_fab_checksum              18174
_olex2_submission_special_instructions 'No special instructions were received'