Remoulding a MOF's pores by auxiliary ligand introduction for stability improvement and highly selective CO<sub>2</sub>-capture.
Zhang, Qing-Qing; Liu, Xiao-Fei; Ma, Lin; Wei, Yong-Sheng; Wang, Zhao-Yang; Xu, Hong; Zang, Shuang-Quan; Chemical communications (Cambridge, England) 54 (2018) 12029–12032; doi:10.1039/c8cc06593d

data_7122381
_publ_section_title
;
 Remoulding a MOF's pores by auxiliary ligand introduction for stability
 improvement and highly selective CO<sub>2</sub>-capture.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12029
_journal_page_last               12032
_journal_paper_doi               10.1039/c8cc06593d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '0.5(C100.02 H56 Co6 N8 O26)'
_chemical_formula_sum            'C50.01 H28 Co3 N4 O13'
_chemical_formula_weight         1069.67
_chemical_name_systematic        Co-pydc-TPB-activated
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.08 svn.r3312 for OlexSys, GUI svn.r5203)
;
_audit_update_record
;
2018-06-25 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.3406(2)
_cell_length_b                   14.3406(2)
_cell_length_c                   14.1626(4)
_cell_measurement_reflns_used    4500
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3780
_cell_measurement_theta_min      3.5380
_cell_volume                     2522.37(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 1.000
_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    -12.00  51.00   0.50    0.50    --    0.00  77.00-150.00  126
  2  \w    -15.00  12.00   0.50    0.50    --    0.00  38.00  30.00   54
  3  \w     56.00  84.00   0.50    0.50    --    0.00  77.00-150.00   56
  4  \w     24.00 119.00   0.50    4.00    --   95.20 -61.00-120.00  190
  5  \w     12.00 107.00   0.50    4.00    --   95.20 -45.00 -30.00  190
  6  \w      9.00  98.00   0.50    4.00    --   95.20 -61.00 -30.00  178
  7  \w     40.00 117.00   0.50    4.00    --   95.20 -82.00-120.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0070226000
_diffrn_orient_matrix_UB_12      -0.0212469000
_diffrn_orient_matrix_UB_13      0.1071371000
_diffrn_orient_matrix_UB_21      -0.0581741000
_diffrn_orient_matrix_UB_22      -0.1220951000
_diffrn_orient_matrix_UB_23      -0.0187498000
_diffrn_orient_matrix_UB_31      0.1093347000
_diffrn_orient_matrix_UB_32      0.0039912000
_diffrn_orient_matrix_UB_33      -0.0031314000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9154
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.490
_diffrn_reflns_theta_min         3.559
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.195
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 562 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.008(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1526
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0595
_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^)+(0.1033P)^2^+3.9798P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    0.930
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                1414
_reflns_number_total             1526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06593d2.cif
_cod_data_source_block           Co-pydc-TPB-activated
_cod_depositor_comments
'Adding full bibliography for 7122380--7122382.cif.'
_cod_original_cell_volume        2522.37(10)
_cod_database_code               7122381
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N S Fe F'
_shelx_estimated_absorpt_t_max   0.495
_shelx_estimated_absorpt_t_min   0.495
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Shared sites
{C14, N2}
3. Restrained distances
 C6-C2
 1.38 with sigma of 0.02
 N1-C2
 1.32 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C14) = Uanis(N2)
5. Others
 Fixed Sof: H1(0.16667) C14(0.335) C2(0.5) H2(0.5) C6(0.5) C4(0.5) H4(0.5)
 C3(0.5) H3(0.5) C5(0.5) H5(0.5) N2(0.16667)
6.a Ternary CH refined with riding coordinates:
 O1(H1)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C2(H2), C4(H4), C3(H3), C11(H11), C9(H9), C5(H5)
;
_shelx_fab_checksum              13535
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.322
_oxdiff_exptl_absorpt_empirical_full_min 0.642