Pyridine polymer tubular structures connected with polyoxometalates as bifunctional electrocatalysts for water splitting.
Wang, Jihua; Li, Hui; Gong, Lige; Dong, Limin; Gu, Yunhao; Wang, Meijia; Yang, BingHe; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3456–3466; doi:10.1039/d4dt02612h

data_7717747
_publ_section_title
;
 Pyridine polymer tubular structures connected with polyoxometalates as
 bifunctional electrocatalysts for water splitting.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3456
_journal_page_last               3466
_journal_paper_doi               10.1039/d4dt02612h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'Mo12 O40 P, 2(C5 H5 N), C4 H4 N2'
_chemical_formula_sum            'C14 H14 Mo12 N4 O40 P'
_chemical_formula_weight         2060.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2jghcw
_audit_creation_date             2023-12-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-03-05 deposited with the CCDC.	2024-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.907(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.1937(5)
_cell_length_b                   13.9195(6)
_cell_length_c                   12.8752(7)
_cell_measurement_reflns_used    5216
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.24
_cell_volume                     2158.96(17)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16677
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.516
_exptl_absorpt_correction_T_max  0.0452
_exptl_absorpt_correction_T_min  0.0213
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0810 before and 0.0594 after correction.
The Ratio of minimum to maximum transmission is 0.4712.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    3.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1930.0
_refine_diff_density_max         5.575
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.291
_refine_ls_extinction_coef       0.0008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4425
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+53.2084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.1993
_reflns_number_gt                3601
_reflns_number_total             4425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt02612h2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7717747--7717750.cif.'
_cod_database_code               7717747
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 P1, O20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O20
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'