A series of isostructural polyoxometalate-based metal-organic frameworks of 3,5-bis(1',2',4'-triazol-1'-yl)pyridine: synthesis, structures and electrocatalytic properties.
Xie, Tinghui; Wang, Xinfang; Cao, Tingting; Huang, Zuogang; Yu, Huaguang; Dalton transactions (Cambridge, England : 2003) 54 (2025) 903–907; doi:10.1039/d4dt02945c

data_1573454
_publ_section_title
;
 A series of isostructural polyoxometalate-based metal-organic frameworks
 of 3,5-bis(1',2',4'-triazol-1'-yl)pyridine: synthesis, structures and
 electrocatalytic properties.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              903
_journal_page_last               907
_journal_paper_doi               10.1039/d4dt02945c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C18 H22 Mo8 N14 Ni2 O30, 4(H2 O)'
_chemical_formula_sum            'C18 H30 Mo8 N14 Ni2 O34'
_chemical_formula_weight         1871.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-07-28
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-28 deposited with the CCDC.	2024-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7082(12)
_cell_length_b                   16.2936(12)
_cell_length_c                   17.7195(13)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.24
_cell_volume                     4535.2(6)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            153894
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.943
_diffrn_reflns_theta_min         2.136
_exptl_absorpt_coefficient_mu    3.064
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4759
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1186 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.6382.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.741
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.00053(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5398
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0170
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5248
_reflns_number_total             5398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02945c2.cif
_cod_data_source_block           2_CCDC2
_cod_depositor_comments
'Adding full bibliography for 1573452--1573454.cif.'
_cod_original_formula_sum        'C18 H22 Mo8 N14 Ni2 O30, 4(H2 O)'
_cod_database_code               1573454
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Restrained distances
 H2B-H16A
 2.1 with sigma of 0.01
 Ni1-H1A \\sim Ni1-H1B
 with sigma of 0.02
 Ni1-H2A \\sim Ni1-H2B
 with sigma of 0.02
2.a Riding coordinates:
 O17(H17A)
2.b Free rotating group:
 O2(H2A,H2B), O1(H1A,H1B), O16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C2(H2), C7(H7), C8(H8), C1(H1), C6(H6), C4(H4)
;
_shelx_res_checksum              33520
_olex2_submission_special_instructions 'No special instructions were received'