Integrating pillared-layer strategy and pore-space partition method to construct multicomponent MOFs for C2H2/CO2 separation.
Liu, Lizhen; Yao, Zizhu; Ye, Yingxiang; Yang, Yike; Lin, Quanjie; Zhang, Zhangjing; O'Keeffe, Michael; Xiang, Shengchang; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00612

data_4134921
_publ_section_title
;
 Integrating pillared-layer strategy and pore-space partition method to
 construct multicomponent MOFs for C2H2/CO2 separation.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00612
_journal_year                    2020
_chemical_formula_moiety         'C52 H30 Co4.5 N7 O17.5'
_chemical_formula_sum            'C52 H30 Co4.5 N7 O17.5'
_chemical_formula_weight         1298.01
_space_group_crystal_system      tetragonal
_space_group_IT_number           118
_space_group_name_Hall           'P -4 -2n'
_space_group_name_H-M_alt        'P -4 n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.7735(5)
_cell_length_b                   21.7735(5)
_cell_length_c                   39.2031(16)
_cell_measurement_reflns_used    7208
_cell_measurement_temperature    294.08(17)
_cell_measurement_theta_max      26.6000
_cell_measurement_theta_min      3.6070
_cell_volume                     18585.6(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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_environment      air
_diffrn_ambient_temperature      294.08(17)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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     35.00  96.20   0.30   41.50    --   10.21 178.00 150.00  204
  2  \w     34.00  97.00   0.30   41.50    --   10.21-178.00-120.00  210
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0122572000
_diffrn_orient_matrix_UB_12      -0.0083903000
_diffrn_orient_matrix_UB_13      0.0161183000
_diffrn_orient_matrix_UB_21      0.0267436000
_diffrn_orient_matrix_UB_22      -0.0174905000
_diffrn_orient_matrix_UB_23      0.0034835000
_diffrn_orient_matrix_UB_31      0.0139662000
_diffrn_orient_matrix_UB_32      0.0261615000
_diffrn_orient_matrix_UB_33      0.0074687000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1080
_diffrn_reflns_av_unetI/netI     0.1652
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            57034
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.344
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    0.928
_exptl_crystal_description       block
_exptl_crystal_F_000             5220
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.375
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Flack x determined using 2597 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.49(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         18187
_refine_ls_number_restraints     776
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.0903
_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^)+(0.1453P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2385
_refine_ls_wR_factor_ref         0.2754
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.921
_reflns_Friedel_fraction_max     0.911
_reflns_number_gt                8914
_reflns_number_total             18187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00612_si_002.cif
_cod_data_source_block           FJU-6-TATB
_cod_original_cell_volume        18585.7(11)
_cod_original_formula_sum        'C52 H30 Co4.50 N7 O17.50'
_cod_database_code               4134921
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'c1 h1 o1 n1 co1'
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.975
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C65-C70 \\sim C54-C38 \\sim C104-N25
 with sigma of 0.02
3. Rigid bond restraints
 O3, O1AA, O1, C4, O15, N25, O2AA, C65, C104, C3, C70, C38, C54, C66, O21, O24,
  O12, O17, O2, O20, O10, O34, O5, C19, C27, C57, C63, C15, O8, C31, C41, O16,
 O11, O23, N9, C40, C59, C22, C29, C44, C2AA, C45, C55, C75, C62, C137, C58,
 C102, C37, C50, C9, C1AA, C52, C73, C39, C72, C49, C77, C6, C36, N32, C42, C33,
  C43, N8, C47, N14, N46, C68, C85, N35, C10, C12, C11, C0AA, C24, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O16, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O3 \\sim O1AA \\sim O1 \\sim C4 \\sim O15 \\sim N25 \\sim O2AA \\sim C65 \\sim
C104 \\sim C3 \\sim C70 \\sim C38 \\sim C54 \\sim C66 \\sim O21 \\sim O24 \\sim
O12 \\sim O17 \\sim O2 \\sim O20 \\sim O10 \\sim O34 \\sim O5 \\sim C19 \\sim
C27 \\sim C57 \\sim C63 \\sim C15 \\sim O8 \\sim C31 \\sim C41 \\sim O16 \\sim
O11 \\sim O23 \\sim N9 \\sim C40 \\sim C59 \\sim C22 \\sim C29 \\sim C44 \\sim
C2AA \\sim C45 \\sim C55 \\sim C75 \\sim C62 \\sim C137 \\sim C58 \\sim C102
\\sim C37 \\sim C50 \\sim C9 \\sim C1AA \\sim C52 \\sim C73 \\sim C39 \\sim C72
\\sim C49 \\sim C77 \\sim C6 \\sim C36 \\sim N32 \\sim C42 \\sim C33 \\sim C43
\\sim N8 \\sim C47 \\sim N14 \\sim N46 \\sim C68 \\sim C85 \\sim N35 \\sim C10
\\sim C12 \\sim C11 \\sim C0AA \\sim C24 \\sim C7: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
O16 \\sim C15: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O2AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C19) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C41) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C2AA) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(N14)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(O1AA) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O34) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(N25) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C65) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C43) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C2AA(H2AA), C36(H36), C37(H37), C62(H62), C39(H39), C72(H72),
 C137(H137), C44(H44), C45(H45), C49(H49), C50(H50), C52(H52), C55(H55),
 C58(H58), C65(H65), C70(H70), C73(H73), C75(H75), C77(H77), C102(H102),
 C104(H104), C12(H12), C0AA(H0AA), C24(H24), C11(H11), C6(H6), C1AA(H1AA),
 C9(H9), C38(H38)
5.b Fitted hexagon refined as free rotating group:
 C40(C62,C39,C33,C72,C137), C47(N14,C68,N35,C85,N46), C10(C12,C0AA,C7,C24,C11)
;
_shelx_res_checksum              68831
_shelx_hkl_checksum              17679
_shelx_fab_checksum              38948
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.350
_oxdiff_exptl_absorpt_empirical_full_min 0.719