Boosting alkaline hydrogen evolution via cobalt functionalization of organic-inorganic hybrid germanoniobate electrocatalysts
Jin, Xinrong; Li, Jin-Yang; Wang, Yong-Jiang; Sun, Yan-Qiong; Li, Xin-Xiong; Zheng, Shou-Tian; CrystEngComm  (2025) –; doi:10.1039/D5CE00954E

data_7251275
_publ_section_title
;
 Boosting alkaline hydrogen evolution via cobalt functionalization of
 organic-inorganic hybrid germanoniobate electrocatalysts
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00954E
_journal_year                    2025
_chemical_formula_moiety
'Ge4 Na3 Nb16 O60, Na O6, 5(O), 4(C2 H10 N2), C2 H9 N2'
_chemical_formula_sum            'C10 H49 Ge4 N10 Na4 Nb16 O71'
_chemical_formula_weight         3314.47
_chemical_name_common            CGeNNaNbO
_chemical_name_systematic        {Ge4Nb16}
_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   geom
_audit_creation_date             2025-09-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-09-19 deposited with the CCDC.	2025-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.428(2)
_cell_angle_beta                 99.138(2)
_cell_angle_gamma                98.546(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8461(9)
_cell_length_b                   14.2158(10)
_cell_length_c                   21.6549(15)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    170
_cell_measurement_theta_max      25.045
_cell_measurement_theta_min      2.431
_cell_volume                     4159.5(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            119674
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.045
_diffrn_reflns_theta_max         25.045
_diffrn_reflns_theta_min         1.906
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.669
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1041 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.7069.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.646
_exptl_crystal_description       block
_exptl_crystal_F_000             3150
_exptl_crystal_preparation       1
_exptl_crystal_recrystallization_method 1
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.135
_refine_diff_density_min         -1.908
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1059
_refine_ls_number_reflns         14711
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+49.1009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13239
_reflns_number_total             14711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00954e2.cif
_cod_data_source_block           a
_cod_database_code               7251275
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.710
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O63) \\sim Ueq, Uanis(O62) \\sim Ueq, Uanis(O61) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.001
Uanis(O56) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(N2) \\sim Ueq, Uanis(O62A) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(O57) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
3. Others
 Fixed Sof: O60(0.5) O62(0.5) O60A(0.5) O62A(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2D,H2E), C3(H3D,H3E), C4(H4D,H4E), C6(H6D,H6E), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10D,H10E)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5)
4.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C), N5(H5A,
 H5B,H5C), N6(H6A,H6B,H6C), N7(H7C,H7D,H7E), N8(H8C,H8D,H8E), N9(H9C,H9D,H9E),
 N10(H10A,H10B,H10C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              52502
_shelx_fab_checksum              54621
_olex2_submission_special_instructions 'No special instructions were received'