Polyoxometalate-based metal–organic supramolecular architectures derived from two new pyrimidine-amide ligands as supercapacitors and multifunctional electrochemical sensors
Wang, Xiu-Li; Lu, Jun-Jun; Lin, Hong-Yan; Liu, Qian-Qian; Chen, Ke-Ke; New Journal of Chemistry 47 (2023) 17051–17059; doi:10.1039/D3NJ02544F

data_7062624
_publ_section_title
;
 Polyoxometalate-based metal--organic supramolecular architectures derived
 from two new pyrimidine-amide ligands as supercapacitors and
 multifunctional electrochemical sensors
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17051
_journal_page_last               17059
_journal_paper_doi               10.1039/D3NJ02544F
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety
'C22 H20 Cl Cu Mo12 N8 O42 P, 3(H2 O), 2.7[H2O]'
_chemical_formula_sum            'C22 H31.4 Cl Cu Mo12 N8 O47.7 P'
_chemical_formula_weight         2452.35
_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             2023-07-23
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-24 deposited with the CCDC.	2023-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                111.2700(10)
_cell_angle_beta                 91.2990(10)
_cell_angle_gamma                113.7070(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8989(4)
_cell_length_b                   14.0884(4)
_cell_length_c                   18.8508(5)
_cell_measurement_reflns_used    9161
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.090
_cell_measurement_theta_min      2.293
_cell_volume                     2865.34(15)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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 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 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0557
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            100629
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.117
_diffrn_reflns_theta_min         1.916
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.082
_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            'greenish green'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2278
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         11352
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0162P)^2^+6.8813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9935
_reflns_number_total             11352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02544f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7062623--7062624.cif.'
_cod_original_cell_volume        2865.34(14)
_cod_database_code               7062624
_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. Restrained distances
 C16-C15 \\sim C8-C16 \\sim C8-C13 \\sim N8-C13 \\sim N8-C14 \\sim C15-C14
 with sigma of 0.02
3. Rigid bond restraints
 N8, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, C8, C13, N8, C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu1, Cl1, N1, N9, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Sof(O1WB)=Sof(H1WA)=Sof(H1WB)=1-FVAR(1)
 Sof(O1WA)=Sof(H1WC)=Sof(H1WD)=FVAR(1)
6.a Riding coordinates:
 O1WA(H1WC,H1WD)
6.b Free rotating group:
 O3W(H3WA,H3WB), O2W(H2WA,H2WB), O1WB(H1WA,H1WB)
6.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C17(H17A,H17B)
6.d Aromatic/amide H refined with riding coordinates:
 N7(H7), N4(H4), C23(H23), C22(H22), C21(H21), C8(H8), C5(H5), C12(H12),
 C16(H16), C9(H9), C11(H11), C3(H3), C14(H14), C10(H10), C4(H4A), C13(H13)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36520
_shelx_fab_checksum              79384
_olex2_submission_special_instructions 'No special instructions were received'