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_7244026
_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         'C13 H30 Co2 Mo6 N6 Na O31.5 Te, 3.5(H2 O)'
_chemical_formula_sum            'C13 H37 Co2 Mo6 N6 Na O35 Te'
_chemical_formula_weight         1681.57
_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_block_doi                 10.5517/ccdc.csd.cc281pbc
_audit_creation_date             2021-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2021-12-07 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.5020(10)
_cell_angle_beta                 95.7840(10)
_cell_angle_gamma                112.6870(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3059(3)
_cell_length_b                   10.2707(4)
_cell_length_c                   27.0831(10)
_cell_measurement_reflns_used    5234
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.433
_cell_measurement_theta_min      2.244
_cell_volume                     2117.91(14)
_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      296.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.984
_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  0.0405
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            39735
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.127
_diffrn_reflns_theta_min         1.513
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.279
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0651 before and 0.0272 after correction.
The Ratio of minimum to maximum transmission is 0.8680.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.637
_exptl_crystal_description       block
_exptl_crystal_F_000             1612
_refine_diff_density_max         1.123
_refine_diff_density_min         -1.962
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         10164
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0379P)^2^+10.0032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7874
_reflns_number_total             10164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01419f2.cif
_cod_data_source_block           2_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7244020--7244026.cif.'
_cod_database_code               7244026
_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
 C5A-C6A
 2.4 with sigma of 0.02
 N4A-C10A = C10A-C5A
 1.4 with sigma of 0.02
 Co1-H5A \\sim Co1-H5B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O38) \\sim Ueq, Uanis(O39) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C2A) \\sim Ueq,
Uanis(C6A) \\sim Ueq, Uanis(N4A) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C5A)
\\sim Ueq, Uanis(N2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O37A) \\sim Ueq, Uanis(O37) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O34) \\sim Ueq, Uanis(O35) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 N2, N4, C2, C4, C5, C6, C10, C13, C13A, C4A, C2A, C6A, N4A, C10A, C5A, N2A, N6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(O37A)=Sof(H37C)=Sof(H37D)=Sof(C10A)=Sof(H10A)=Sof(N4A)=Sof(C6A)=Sof(H6A)=
 Sof(C5A)=Sof(H5AA)=Sof(N2A)=Sof(H2AC)=1-FVAR(1)
 Sof(N4)=Sof(C6)=Sof(H6)=Sof(N2)=Sof(H2)=Sof(C5)=Sof(H5)=Sof(C10)=Sof(H10)=
 Sof(O37)=Sof(H37A)=Sof(H37B)=FVAR(1)
 Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(2)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C13)=Sof(H13A)=
 Sof(H13B)=FVAR(2)
 Fixed Sof: O35(0.5) H35A(0.5) H35B(0.5) O38(0.5) H38A(0.5) H38B(0.5) O39(0.5)
 H39A(0.5) H39B(0.5) O40(0.5) H40A(0.5) H40B(0.5)
6.a Riding coordinates:
 O5(H5A,H5B), O8(H8A,H8B), O11(H11A,H11B), O20(H20A,H20B), O21(H21A,H21),
 O33(H33A,H33B), O34(H34A,H34B), O35(H35A,H35B), O36(H36A,H36B), O37(H37A,H37B),
  O37A(H37C,H37D), O38(H38A,H38B), O39(H39A,H39B), O40(H40A,H40B)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C13(H13A,H13B), C13A(H13C,H13D), C4A(H4AA,H4AB),
 C2A(H2AA,H2AB)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), N2(H2), C5(H5), C10(H10), C3(H3), C7(H7), C8(H8), C9(H9), C11(H11),
 C10A(H10A), C6A(H6A), C5A(H5AA), N2A(H2AC)
6.d Fitted pentagon refined as free rotating group:
 N4(C6,N2,C5,C10), C10A(N4A,C6A,C5A,N2A)
;
_shelx_res_checksum              14087
_shelx_hkl_checksum              55985
_olex2_submission_special_instructions 'No special instructions were received'