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_7062623
_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         'Mo4 O14, C15 H22 Co N6 O4, H2 O, 3.5[H2O]'
_chemical_formula_sum            'C15 H31 Co Mo4 N6 O22.5'
_chemical_formula_weight         1098.099
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2023-07-11
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.04.26 svn.r751481ca for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2023-07-24 deposited with the CCDC.	2023-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                100.703(3)
_cell_angle_beta                 92.255(3)
_cell_angle_gamma                106.731(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7501(16)
_cell_length_b                   11.7700(17)
_cell_length_c                   13.702(2)
_cell_measurement_reflns_used    1489
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     1623.5(4)
_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 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.9923
_diffrn_measured_fraction_theta_max 0.9923
_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_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0894
_diffrn_reflns_Laue_measured_fraction_full 0.9923
_diffrn_reflns_Laue_measured_fraction_max 0.9923
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9014
_diffrn_reflns_point_group_measured_fraction_full 0.9923
_diffrn_reflns_point_group_measured_fraction_max 0.9923
_diffrn_reflns_theta_full        25.0375
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    2.100
_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    2.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064.026
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.8711
_refine_diff_density_min         -1.6283
_refine_diff_density_rms         0.3367
_refine_ls_d_res_high            0.8397
_refine_ls_d_res_low             13.3982
_refine_ls_goodness_of_fit_ref   1.0425
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     413
_refine_ls_number_reflns         5696
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.0417
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          -0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+11.1925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3925
_reflns_number_total             5696
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj02544f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7062623--7062624.cif.'
_cod_original_formula_sum        'C15 H31 Co1 Mo4 N6 O22.5'
_cod_database_code               7062623
_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
 Co1-H2Wa \\sim Co1-H2Wb
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4.a Free rotating group:
 O2W(H2Wa,H2Wb), O3W(H3Wa,H3Wb)
4.b Rotating group:
 O1W(H1Wa,H1Wb)
4.c Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C9(H9a,H9b), C8(H8a,H8b), C7(H7a,H7b), C6(H6a,H6b)
4.d Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), C1(H1), C15(H15), C14(H14), C13(H13), C3(H3), C2(H2)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 70 electrons were 
found in a volume of 218\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 3.5[H2O] per Formula Unit 
which account for 70 electrons per unit cell.
;
_olex2_submission_special_instructions 'No special instructions were received'