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_7244025
_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         'C26 H43 Co2 N12 O41 P W11, 4.5(H2 O)'
_chemical_formula_sum            'C26 H52 Co2 N12 O45.5 P W11'
_chemical_formula_weight         3431.97
_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.cc282tfm
_audit_creation_date             2021-11-23
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2021-11-30 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0455(16)
_cell_length_b                   14.5002(12)
_cell_length_c                   23.178(2)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.85
_cell_measurement_theta_min      2.26
_cell_volume                     6367.8(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0755
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            96373
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.766
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.420
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1475 before and 0.0532 after correction.
The Ratio of minimum to maximum transmission is 0.5149.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.580
_exptl_crystal_description       block
_exptl_crystal_F_000             6156
_refine_diff_density_max         1.826
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         11829
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0202P)^2^+35.5920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9184
_reflns_number_total             11829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01419f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7244020--7244026.cif.'
_cod_original_formula_sum        'C26 H52 Co2 N12 O45.50 P W11'
_cod_database_code               7244025
_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, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O43)
\\sim Ueq, Uanis(O47) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(O39) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O11(0.5) H11C(0.5) H11D(0.5) O23(0.5) H23A(0.5) H23B(0.5) O43(0.5)
 H43A(0.5) H43B(0.5) O45(0.5) H45A(0.5) H45B(0.5) O47(0.5) H47A(0.5) H47B(0.5)
4.a Riding coordinates:
 O21(H21C,H21D), O25(H25A,H25B), O46(H46A,H46B), O11(H11C,H11D), O23(H23A,
 H23B), O39(H39A,H39B), O43(H43A,H43B), O45(H45A,H45B), O47(H47A,H47B)
4.b Ternary CH refined with riding coordinates:
 N3(H3)
4.c Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), N11(H11A,H11B), C2(H2A,H2B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,
 H10B), C12(H12A,H12B), C13(H13A,H13B), C17(H17A,H17B), C19(H19A,H19B),
 C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B), C25(H25C,H25D)
4.d Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C8(H8), C14(H14), C15(H15), C16(H16), C18(H18),
 C23(H23), C26(H26)
;
_shelx_res_checksum              20473
_shelx_hkl_checksum              72623
_olex2_submission_special_instructions 'No special instructions were received'