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_7244023
_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_absolute_configuration ad
_chemical_formula_moiety         'C52 H70 Cu5 Mo22 N24 O83 P2, 6(H2 O)'
_chemical_formula_sum            'C52 H82 Cu5 Mo22 N24 O89 P2'
_chemical_formula_weight         4957.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc280xv2
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.2769(7)
_cell_length_b                   13.9736(4)
_cell_length_c                   19.3429(6)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.277
_cell_volume                     6291.5(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0440
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45825
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.480
_diffrn_reflns_theta_min         1.700
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.075
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0850 before and 0.0363 after correction.
The Ratio of minimum to maximum transmission is 0.7711.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.617
_exptl_crystal_description       block
_exptl_crystal_F_000             4746
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.527
_refine_diff_density_rms         0.178
_refine_ls_abs_structure_details
;
 Flack x determined using 4905 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         14836
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+2.3720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    0.888
_reflns_Friedel_fraction_max     0.863
_reflns_number_gt                12576
_reflns_number_total             14836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01419f2.cif
_cod_data_source_block           2_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7244020--7244026.cif.'
_cod_database_code               7244023
_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, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N11A-C25A
 2.4 with sigma of 0.02
 N5A-C25A = C25A-N11A
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O47) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(O46) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O46) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(O47) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(N5) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C11A) \\sim Ueq,
Uanis(N5A) \\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(N11A) \\sim Ueq, Uanis(C3A)
\\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 N5, N5A, N11, N11A, C3, C3A, C11, C11A, C21, C23, C23A, C25, C25A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cu3, O45, O46, O47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(H21C)=Sof(H21D)=Sof(C25A)=Sof(H25A)=
 Sof(N5A)=Sof(C23A)=Sof(H23A)=Sof(C3A)=Sof(H3AA)=Sof(N11A)=1-FVAR(1)
 Sof(N5)=Sof(C23)=Sof(H23)=Sof(C3)=Sof(H3A)=Sof(N11)=Sof(C25)=Sof(H25)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H21A)=Sof(H21B)=FVAR(1)
 Fixed Sof: Cu3(0.5) O45(0.5) H45A(0.5) H45B(0.5) O46(0.5) H46A(0.5) H46B(0.5)
 O47(0.5) H47A(0.5) H47B(0.5)
6.a Riding coordinates:
 O30(H30A,H30B), O45(H45A,H45B), O46(H46A,H46B), O47(H47A,H47B), O41(H41A,
 H41B), O43(H43A,H43B), O44(H44A,H44B)
6.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C11A(H11C,H11D), C13(H13A,H13B), C14(H14A,H14B),
 C20(H20A,H20B), C21(H21A,H21B), C21(H21C,H21D)
6.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C23(H23), C3(H3A), C25(H25), N9(H9), C2(H2), C5(H5), C6(H6), C7(H7),
 C10(H10), C12(H12), C15(H15), C17(H17), C18(H18), C19(H19), C22(H22), C24(H24),
  C25A(H25A), C23A(H23A), C3A(H3AA), C26(H26)
6.d Fitted pentagon refined as free rotating group:
 N5(C23,C3,N11,C25), C25A(N5A,C23A,C3A,N11A)
;
_shelx_res_checksum              88215
_shelx_hkl_checksum              7654
_olex2_submission_special_instructions 'No special instructions were received'