A post synthetically modified metal–organic framework as an efficient hydrogen evolution reaction catalyst in all pH conditions
Mondal, Tuhina; Hota, Poulami; Sarkar, Koushik; Debnath, Anup; Shaw, Bikash Kumar; Saha, Shyamal K.; New Journal of Chemistry 47 (2023) 8102–8110; doi:10.1039/D3NJ00791J

data_7062397
_publ_section_title
;
 A post synthetically modified metal--organic framework as an efficient
 hydrogen evolution reaction catalyst in all pH conditions
;
_journal_issue                   17
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8102
_journal_page_last               8110
_journal_paper_doi               10.1039/D3NJ00791J
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C23 H18 N6 Ni O5, 0.74(O)'
_chemical_formula_sum            'C23 H18 N6 Ni O5.74'
_chemical_formula_weight         528.98
_chemical_name_systematic        Niipa
_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
_audit_block_doi                 10.5517/ccdc.csd.cc28m255
_audit_creation_date             2020-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-17 deposited with the CCDC.	2023-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.13(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.828(3)
_cell_length_b                   16.662(5)
_cell_length_c                   17.222(5)
_cell_measurement_reflns_used    5501
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      23.543
_cell_measurement_theta_min      2.369
_cell_volume                     2529.4(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.920
_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  0.0611
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34200
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.715
_diffrn_reflns_theta_min         1.702
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0821 before and 0.0555 after correction. The Ratio of minimum to maximum transmission is 0.9155. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0509
_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^)+(0.1116P)^2^+0.2518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3772
_reflns_number_total             6020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00791j2.cif
_cod_data_source_block           ks0461c_0m_a
_cod_depositor_comments          'Adding full bibliography for 7062397.cif.'
_cod_original_cell_volume        2529.5(14)
_cod_database_code               7062397
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.867
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(O6B)=1-FVAR(1)
 Sof(O6A)=0.5*FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C2(H2), C6(H6), C9(H9), C19(H19), C18(H18), C23(H23), C20(H20),
 C22(H22), C14(H14), C13(H13), C10(H10), C21(H21), C11(H11), C15(H15), C17(H17),
  C16(H16), C12(H12)
;
_shelx_res_checksum              91253
_shelx_hkl_checksum              44507
_olex2_submission_special_instructions 'No special instructions were received'