A series of POM-based compounds by tuning coordination groups and spacers of ligands: electrocatalytic, capacitive and photoelectrocatalytic properties
Sun, Chenxi; Ying, Jun; Zhang, Yanping; Jin, Liang; Tian, Aixiang; Wang, Xiuli; CrystEngComm 24 (2022) 587–600; doi:10.1039/D1CE01419F

data_7244021
_publ_section_title
;
 A series of POM-based compounds by tuning coordination groups and spacers
 of ligands: electrocatalytic, capacitive and photoelectrocatalytic
 properties
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              587
_journal_page_last               600
_journal_paper_doi               10.1039/D1CE01419F
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C52 H62 Co Mo24 N24 O80 Si2, 2(H2 O)'
_chemical_formula_sum            'C52 H66 Co Mo24 N24 O82 Si2'
_chemical_formula_weight         4756.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc27wp2x
_audit_creation_date             2021-11-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6427)
;
_audit_update_record
;
2021-11-30 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.364(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1279(15)
_cell_length_b                   21.743(3)
_cell_length_c                   21.136(3)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.35
_cell_volume                     5444.2(13)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38100
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.253
_diffrn_reflns_theta_min         1.719
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.954
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1056 before and 0.0448 after correction.
The Ratio of minimum to maximum transmission is 0.6721.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.902
_exptl_crystal_description       block
_exptl_crystal_F_000             4530
_refine_diff_density_max         1.053
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         13408
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0083P)^2^+16.0830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11218
_reflns_number_total             13408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01419f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7244020--7244026.cif.'
_cod_original_cell_volume        5444.1(12)
_cod_database_code               7244021
_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
 At 1.5 times of:
  All N(H) groups, All O(H,H) groups
2. Restrained distances
 H41A-O41 = O41-H41B
 0.85 with sigma of 0.02
 H12-N12 = H10-N10
 0.85 with sigma of 0.02
 N6-H6 = N6A-H6A
 0.85 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N5, N6, C11, C13, C25, C13A, N6A, C11A, C25A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C13A)=Sof(H13A)=Sof(N6A)=Sof(H6A)=Sof(C11A)=Sof(H11A)=Sof(C25A)=Sof(H25A)=
 1-FVAR(1)
 Sof(N6)=Sof(H6)=Sof(C11)=Sof(H11)=Sof(C13)=Sof(H13)=Sof(C25)=Sof(H25)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C11(H11), C12(H12A), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C23(H23), C24(H24), C25(H25),
  C13A(H13A), C11A(H11A), C25A(H25A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              86244
_shelx_hkl_checksum              45082
_olex2_submission_special_instructions 'No special instructions were received'