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_7244024
_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
'2(Cr0.5 H3 Mo3 O12), C12 H18 Cu N7 O2, 5(H2 O)'
_chemical_formula_sum            'C12 H34 Cr Cu Mo6 N7 O31'
_chemical_formula_weight         1463.64
_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.cc288v8p
_audit_creation_date             2021-11-07
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-11-30 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                110.6770(10)
_cell_angle_beta                 110.3810(10)
_cell_angle_gamma                98.3070(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2348(7)
_cell_length_b                   13.5570(8)
_cell_length_c                   13.8907(8)
_cell_measurement_reflns_used    4002
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.43
_cell_volume                     1924.4(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.991
_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  0.0195
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14247
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.348
_diffrn_reflns_theta_min         1.686
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.813
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0397 before and 0.0270 after correction.
The Ratio of minimum to maximum transmission is 0.8988.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.526
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_refine_diff_density_max         1.125
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         9516
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0328P)^2^+3.3526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6914
_reflns_number_total             9516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01419f2.cif
_cod_data_source_block           2_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7244020--7244026.cif.'
_cod_original_cell_volume        1924.40(19)
_cod_database_code               7244024
_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 C(H,H,H,H) groups
 At 1.5 times of:
  All N(H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H1-O1 = H8A-O8 = H4-O4 = H16-O16 = H12A-O12 = H6A-O6
 0.85 with sigma of 0.02
 C5A-N5A = N5A-C9A
 1.45 with sigma of 0.02
 H5-N5 = H5A-N5A
 0.85 with sigma of 0.02
 H5A-O29
 2.35 with sigma of 0.02
 H7B-O7 = O7-H7A
 0.85 with sigma of 0.02
 H7A-O25_$1
 2.2 with sigma of 0.02
 H5-H29B
 2.2 with sigma of 0.02
 H5-H29A
 2.2 with sigma of 0.02
 H26A-O26 = O26-H26B
 0.85 with sigma of 0.02
 H20A-O20 = O20-H20B
 0.85 with sigma of 0.02
 H13B-O13 = O13-H13A
 0.85 with sigma of 0.02
 H29B-O29 = O29-H29A
 0.85 with sigma of 0.02
 H27B-O27 = O27-H27A
 0.85 with sigma of 0.02
 H27B-H27A
 1.45 with sigma of 0.02
 C5A-C2A = C2A-N3A
 1.45 with sigma of 0.02
 H13A-H27B
 2.2 with sigma of 0.02
 H15D-O15A = O15A-H15C
 0.85 with sigma of 0.02
 H15A-O15 = O15-H15B
 0.85 with sigma of 0.02
 H6A_$2-H13B
 2.2 with sigma of 0.02
 H15A-H15B = H15D-H15C
 1.45 with sigma of 0.02
 H15D-O25_$3
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N5) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C2A) \\sim Ueq, Uanis(N5A) \\sim Ueq, Uanis(C5A) \\sim Ueq,
Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N3, N3A, N5, N5A, C2, C2A, C5, C5A, C7, C9, C9A, C11, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N3A)=Sof(N5A)=Sof(H5A)=Sof(C2A)=Sof(H2A)=Sof(C5A)=Sof(H5AA)=Sof(H7AA)=
 Sof(H7AB)=Sof(C9A)=Sof(H9A)=Sof(C11A)=Sof(H11C)=Sof(H11D)=1-FVAR(1)
 Sof(N3)=Sof(N5)=Sof(H5)=Sof(C2)=Sof(H2)=Sof(C5)=Sof(H5B)=Sof(H7BC)=Sof(H7BD)=
 Sof(C9)=Sof(H9)=Sof(C11)=Sof(H11A)=Sof(H11B)=FVAR(1)
 Sof(O15A)=Sof(H15C)=Sof(H15D)=1-FVAR(2)
 Sof(O15)=Sof(H15A)=Sof(H15B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C7(H7BC,H7BD), C7(H7AA,H7AB), C11(H11A,H11B), C11A(H11C,H11D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C2A(H2A), C5(H5B), C5A(H5AA), C6(H6), C8(H8), C9(H9), C9A(H9A),
 C10(H10), C12(H12)
;
_shelx_res_checksum              36019
_shelx_hkl_checksum              50157
_olex2_submission_special_instructions 'No special instructions were received'