An ato-Topology Metal-Organic Framework with Large C2H2 Adsorption and C2H2/CO2 Separation Capacity
Wang, Ting; Jiang, Zhi-Jie; Wang, Ying; Wei, Rong-Jia; Zeng, Heng; Lu, Weigang; Li, Dan; Dalton Transactions  (2022) –; doi:10.1039/D2DT02968E

data_7711684
_publ_section_title
;
 An ato-Topology Metal-Organic Framework with Large C2H2 Adsorption and
 C2H2/CO2 Separation Capacity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02968E
_journal_year                    2022
_chemical_formula_moiety
'C16 H12 Co N4 O5, 0.5(O), C2 H6 O, C4 H9 N O, 1[H2O]'
_chemical_formula_sum            'C22 H30 Co N5 O8.5'
_chemical_formula_weight         559.44
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-10-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-31 deposited with the CCDC.	2022-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   41.7037(7)
_cell_length_b                   41.7037(7)
_cell_length_c                   9.8644(2)
_cell_measurement_reflns_used    3926
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.4670
_cell_measurement_theta_min      4.2460
_cell_volume                     14857.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     82.00 193.00   0.50   13.76    --  105.10  39.00 -42.00  222
  2  \w     78.00 121.00   0.50   13.76    --  105.10 -40.00-157.00   86
  3  \w     -3.00  31.00   0.50    3.44    --   -0.90 -82.00  60.00   68
  4  \w    -36.00  32.00   0.50    3.44    --   -0.90 -82.00-150.00  136
  5  \w     76.00 119.00   0.50   13.76    --  105.10  77.00-120.00   86
  6  \w    138.00 194.00   0.50   13.76    --  105.10  77.00-120.00  112
  7  \w     92.00 183.00   0.50   13.76    --  105.10  38.00   0.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16707
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.665
_diffrn_reflns_theta_min         4.240
_exptl_absorpt_coefficient_mu    4.464
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             5256
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         6737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0718
_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^)+(0.1239P)^2^+41.3451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1962
_refine_ls_wR_factor_ref         0.2053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5501
_reflns_number_total             6737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02968e2.cif
_cod_data_source_block           as-synthesized_jnu-7_100k
_cod_original_cell_volume        14857.7(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C22 H30 Co N5 O8.50'
_cod_database_code               7711684
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.664
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O6(0.5)
3.a Rotating group:
 O5(H5A,H5B)
3.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C13(H13), C14(H14), C15(H15), C16(H16)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C)
3.e Idealised tetrahedral OH refined as rotating group:
 O7(H7A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 168 electrons were 
found in a volume of 4308\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[H2O] per Asymmetric Unit 
which account for 180 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12754
_shelx_hkl_checksum              34828
_shelx_fab_checksum              42048
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;