Organic-inorganic hybrid Co-containing polyoxoniobates as hydrogen evolution catalysts in alkaline media.
Chen, Chun-Xia; Duan, Shui-Lin; Zhang, Xiao-Yue; Sun, Rong-Zhi; Cai, Ping-Wei; Sun, Cai; Zheng, Shou-Tian; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3591–3596; doi:10.1039/d4dt03071k

data_7717809
_publ_section_title
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 Organic-inorganic hybrid Co-containing polyoxoniobates as hydrogen
 evolution catalysts in alkaline media.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3591
_journal_page_last               3596
_journal_paper_doi               10.1039/d4dt03071k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'H8 K2 Nb8 O32 Ti2, 2(C6 H24 Co N6), 8(H2 O)'
_chemical_formula_sum            'C12 H72 Co2 K2 N12 Nb8 O40 Ti2'
_chemical_formula_weight         2059.810
_chemical_name_systematic        Co2-Ti2Nb8
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-12-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-16 deposited with the CCDC.	2025-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.361(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.882(3)
_cell_length_b                   21.468(5)
_cell_length_c                   12.867(3)
_cell_measurement_reflns_used    7555
_cell_measurement_temperature    170
_cell_measurement_theta_max      24.951
_cell_measurement_theta_min      2.271
_cell_volume                     2727.4(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX 3'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.9893
_diffrn_measured_fraction_theta_max 0.9893
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.9893
_diffrn_reflns_Laue_measured_fraction_max 0.9893
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11168
_diffrn_reflns_point_group_measured_fraction_full 0.9893
_diffrn_reflns_point_group_measured_fraction_max 0.9893
_diffrn_reflns_theta_full        24.9685
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.85
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.743
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0574 before and 0.0282 after correction.
The Ratio of minimum to maximum transmission is 0.8226.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.508
_exptl_crystal_description       cube
_exptl_crystal_F_000             1995.354
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.4565
_refine_diff_density_min         -0.4067
_refine_diff_density_rms         0.0936
_refine_ls_d_res_high            0.8419
_refine_ls_d_res_low             11.0296
_refine_ls_goodness_of_fit_ref   1.0669
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    17
_refine_ls_number_parameters     407
_refine_ls_number_reflns         4735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0669
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          -0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+2.8117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0414
_refine_ls_wR_factor_ref         0.0422
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -11
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              -8
_reflns_number_gt                4483
_reflns_number_total             4735
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt03071k2.cif
_cod_data_source_block           Co2-Ti2Nb8
_cod_depositor_comments
'Adding full bibliography for 7717809--7717810.cif.'
_cod_database_code               7717809
_olex2_refinement_description
;
1.a Free rotating group:
 O15(H15a,H15b), O17(H17a,H17b), O18(H18a,H18b), O19(H19a,H19b)
1.b Rotating group:
 O16(H16a,H16b)
1.c Secondary CH2 refined with riding coordinates:
 N1(H1a,H1b), N2(H2a,H2b), N3(H3a,H3b), N4(H4a,H4b), N5(H5a,H5b), N6(H6a,H6b),
 C1(H1c,H1d), C2(H2c,H2d), C3(H3c,H3d), C4(H4c,H4d), C5(H5c,H5d), C6(H6c,H6d)
;
_olex2_submission_special_instructions 'No special instructions were received'