A 2D flexible cobalt-MOF: reversible solid-state structural transformation, two-step and gate-opening adsorption behaviour and selective adsorption of C2H2 over CO2 and CH4
Wang, Shan-Shan; Liang, Yu-Jie; Guo, Wei; Yin, Yue; Li, Xiao-Yu; Xu, Quan-Qing; Zhu, Ai-Xin; Huang, Bo; Dalton Transactions  (2023) –; doi:10.1039/D3DT00478C

data_7713210
_publ_section_title
;
 A 2D flexible cobalt-MOF: reversible solid-state structural
 transformation, two-step and gate-opening adsorption behaviour and
 selective adsorption of C2H2 over CO2 and CH4
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00478C
_journal_year                    2023
_chemical_formula_moiety         'C56 H36 Co3 N4 O12, [3DMF+2.5H2O]'
_chemical_formula_sum            'C65 H62 Co3 N7 O17.5'
_chemical_formula_weight         1398.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-05-24 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.21(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.078(5)
_cell_length_b                   23.525(5)
_cell_length_c                   27.050(12)
_cell_measurement_reflns_used    431
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      4.41
_cell_volume                     14102(8)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'DIAMOND (Brandenburg, 1999)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1190
_diffrn_reflns_av_unetI/netI     0.0896
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62790
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.041
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 2001)'
_exptl_crystal_colour            blue-purple
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             4616
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.220
_refine_diff_density_max         1.643
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         12396
_refine_ls_number_restraints     398
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0913
_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^)+(0.1458P)^2^+31.3044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2501
_refine_ls_wR_factor_ref         0.2649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9264
_reflns_number_total             12396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00478c2.cif
_cod_data_source_block           Co-MOF-alpha
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7713210
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.796
_shelx_estimated_absorpt_t_max   0.853
_shelx_res_checksum              16993
_smtbx_masks_special_details
;
The 1097 electrons were removed from the unit-cell 
contents by using SQUEEZE process, which is equivalent
to 137 electrons per asymmetric unit. As the formula 
unit is composed of one asymmetric units, this implies 
that 137 electrons should be associated with the 
disordered solvent. The total electrons (145 electrons)
with the contribution of disorder solvents including
three DMF and two and a half water molecules are almost in 
accordance with the SQUEEZE results. TG analysis also indicate
that this compound contains three molecules of DMF and
2.5 water molecules per formula unit. 
;
_smtbx_masks_void_probe_radius   1.20
_smtbx_masks_void_truncation_radius 1.20
_shelx_hkl_checksum              91280
_shelx_fab_checksum              47612