Co-based MOF heterogeneous catalyst for efficient degradation of organic dye via peroxymonosulfate activation
Xie, Wei; Yuan, Yuan; Wang, Jia-Jun; Zhang, Shuran; Xu, Guangjuan; Jiang, Nan; Xu, Yanhong; Su, Zhong-Min; Dalton Transactions  (2023) –; doi:10.1039/D3DT01783D

data_7713993
_publ_section_title
;
 Co-based MOF heterogeneous catalyst for efficient degradation of organic
 dye via peroxymonosulfate activation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01783D
_journal_year                    2023
_chemical_formula_moiety
'C20 H13 Co2 N2 O7, C4 H9 N O, 2[C4H9NO], 0.75[H2O]'
_chemical_formula_sum            'C32 H41.5 Co2 N5 O10.75'
_chemical_formula_weight         786.06
_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
_audit_creation_date             2023-09-12
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-14 deposited with the CCDC.	2023-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.059(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.649(7)
_cell_length_b                   12.876(6)
_cell_length_c                   17.677(8)
_cell_measurement_reflns_used    3737
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     3405(3)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15277
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.530
_exptl_absorpt_coefficient_mu    1.041
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1634
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.0056(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5940
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0677
_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^)+(0.1176P)^2^+1.3716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1872
_refine_ls_wR_factor_ref         0.2006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4343
_reflns_number_total             5940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01783d2.cif
_cod_data_source_block           x
_cod_original_formula_sum        'C32 H41.50 Co2 N5 O10.75'
_cod_database_code               7713993
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.819
_shelx_estimated_absorpt_t_min   0.788
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16-O8
 1.22 with sigma of 0.005
 C16-C17
 1.497 with sigma of 0.005
 C16-N5
 1.322 with sigma of 0.005
 C18-N5
 1.459 with sigma of 0.005
 C19-N5
 1.459 with sigma of 0.005
3. Restrained planarity
 O8, N5, C16, C17, C18, C19
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Free rotating group:
 O8(N5,C16,C17,C18,C19)
5.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
5.c Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15),
 C22(H22), C20(H20)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 412 electrons were 
found in a volume of 1261\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C4H9NO], 0.75[H2O] per Unit Cell 
which account for 414 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              6396
_shelx_fab_checksum              52767
_olex2_submission_special_instructions 'No special instructions were received'