Iron-doped novel Co-based metal-organic frameworks for preparation of bifunctional catalysts with amorphous structure for OER/HER in alkaline solution
Dai, Siyu; Liu, Yuqi; Mei, Yunjie; Hu, Jue; Wang, Kaiming; Li, Yanghua; Jin, Nanhao; Wang, Xinying; Luo, Huilong; Li, Wei; Dalton Transactions  (2022) –; doi:10.1039/D2DT01837C

data_7711242
_publ_section_title
;
 Iron-doped novel Co-based metal-organic frameworks for preparation of
 bifunctional catalysts with amorphous structure for OER/HER in alkaline
 solution
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01837C
_journal_year                    2022
_chemical_formula_moiety         'C26 H16 Co N6 O5, 2(C3 H7 N O)'
_chemical_formula_sum            'C32 H30 Co N8 O7'
_chemical_formula_weight         697.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-26 deposited with the CCDC.	2022-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.414(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.942(2)
_cell_length_b                   13.1857(19)
_cell_length_c                   18.636(3)
_cell_measurement_reflns_used    2423
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      22.79
_cell_measurement_theta_min      2.20
_cell_volume                     3189.4(8)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0666
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15957
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         1.569
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6589
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0871 before and 0.0503 after correction.
The Ratio of minimum to maximum transmission is 0.8837.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       block
_exptl_crystal_F_000             1444
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         5615
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0773P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3404
_reflns_number_total             5615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01837c2.cif
_cod_data_source_block           ww
_cod_original_cell_volume        3189.5(8)
_cod_database_code               7711242
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.937
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O7-C30
 1.22 with sigma of 0.02
 C30-N8
 1.35 with sigma of 0.02
 N8-C31
 1.43 with sigma of 0.02
 N8-C32
 1.43 with sigma of 0.02
 N8-O7
 2.31 with sigma of 0.02
 C30A-O7A
 1.22 with sigma of 0.02
 N8A-C30A
 1.35 with sigma of 0.02
 C31A-C30A
 2.37 with sigma of 0.02
 N8A-O7A
 2.35 with sigma of 0.02
 C32A-C30A
 2.37 with sigma of 0.02
 N8A-C31A
 1.45 with sigma of 0.02
3. Rigid bond restraints
 N8, C31, C32, O7, C30, O7A, C30A, N8A, C31A, C32A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N8 \\sim C31 \\sim C32 \\sim O7 \\sim C30 \\sim O7A \\sim C30A \\sim N8A \\sim
C31A \\sim C32A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O7) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(O7A) \\sim Ueq, Uanis(C30A) \\sim Ueq,
Uanis(N8A) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C32A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(O7A)=Sof(C30A)=Sof(H30A)=Sof(N8A)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=
 Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(N8)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(H32C)=Sof(O7)=Sof(C30)=Sof(H30)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C17(H17), C19(H19), C12(H12), C16(H16), C24(H24), C7(H7), C9(H9),
 C10(H10), C15(H15), C6(H6), C3(H3), C26(H26), C25(H25), C4(H4), C22(H22),
 C29(H29), C30(H30), C30A(H30A)
6.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C31A(H31D,H31E,H31F), C32A(H32D,H32E,H32F)
;
_shelx_res_checksum              44672
_shelx_hkl_checksum              96043
_olex2_submission_special_instructions 'No special instructions were received'