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_4134919
_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         'C55 H33 Co4.5 N4 O17.5'
_chemical_formula_sum            'C55 H33 Co4.5 N4 O17.5'
_chemical_formula_weight         1295.04
_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     iterative
_audit_creation_date             2018-09-05
_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                   21.8423(5)
_cell_length_b                   21.8423(5)
_cell_length_c                   39.3731(18)
_cell_measurement_reflns_used    4927
_cell_measurement_temperature    291.10(10)
_cell_measurement_theta_max      72.6180
_cell_measurement_theta_min      4.0250
_cell_volume                     18784.4(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.10(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.973
_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   -118.00  -9.00   1.00   15.00    --  -41.45 -77.00  30.00  109
  2  \w    -29.00 129.00   1.00   15.00    --   41.45   0.00  60.00  158
  3  \w     33.00  63.00   1.00   32.50    --  106.36 -45.00 -60.00   30
  4  \w     44.00 103.00   1.00   32.50    --  106.36 -94.00  30.00   59
  5  \w     31.00  82.00   1.00   32.50    --  106.36 -30.00  30.00   51
  6  \w     41.00  85.00   1.00   32.50    --  106.36 -30.00 150.00   44
  7  \w     34.00  98.00   1.00   32.50    --  106.36 -45.00   0.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0422202000
_diffrn_orient_matrix_UB_12      0.0463255000
_diffrn_orient_matrix_UB_13      0.0179630000
_diffrn_orient_matrix_UB_21      0.0004052000
_diffrn_orient_matrix_UB_22      -0.0405447000
_diffrn_orient_matrix_UB_23      0.0320107000
_diffrn_orient_matrix_UB_31      0.0565392000
_diffrn_orient_matrix_UB_32      -0.0342749000
_diffrn_orient_matrix_UB_33      -0.0136126000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.2249
_diffrn_reflns_av_unetI/netI     0.2299
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            50756
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.808
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pinkish black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    0.916
_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         1.612
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Flack x determined using 1942 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.54(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         16037
_refine_ls_number_restraints     910
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.1809
_refine_ls_R_factor_gt           0.0970
_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^)+(0.1185P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2283
_refine_ls_wR_factor_ref         0.2793
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.909
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                7107
_reflns_number_total             16037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00612_si_002.cif
_cod_data_source_block           FJU-6
_cod_original_cell_volume        18784.3(12)
_cod_original_formula_sum        'C55 H33 Co4.50 N4 O17.50'
_cod_database_code               4134919
_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   0.976
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C24-C27
 1.23 with sigma of 0.02
 C13_$1-C8_$1
 1.429 with sigma of 0.02
 C1-C2
 1.3 with sigma of 0.02
 O12-C1
 1.2 with sigma of 0.02
 C37-C38
 1.4 with sigma of 0.02
 C12-C13 = C12-C11 = C12-C14
 1.38 with sigma of 0.02
 C18-C17 = C14-C12
 1.4 with sigma of 0.02
 C28-C30
 2.78 with sigma of 0.02
 C32-C29
 2.78 with sigma of 0.02
 N1-C31
 2.78 with sigma of 0.02
 C21-C10
 1.5 with sigma of 0.02
 C13_$1-C8_$1 \\sim C13_$1-C12_$1 \\sim C12_$1-C11_$1 \\sim C10_$1-C11_$1 \\sim
C9_$1-C10_$1 ~
 C9_$1-C8_$1
 with sigma of 0.02
 N2-C36 \\sim N2-C34 \\sim C34-C35 \\sim C38-C35 \\sim C37-C36 \\sim C37-C38
 with sigma of 0.02
 N1-C28 \\sim N1-C29 \\sim C30-C29 \\sim C31-C30 \\sim C32-C31 \\sim C32-C28
 with sigma of 0.02
3. Restrained planarity
 C8_$1, C13_$1, C12_$1, C11_$1, C10_$1, C9_$1
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C26 \\sim C25 \\sim C22 \\sim C21 \\sim C23 \\sim C24: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C12 \\sim C13 \\sim C8 \\sim C9 \\sim C10 \\sim C11: within 1.7A with sigma of
0.0051 and sigma for terminal atoms of 0.01
C14 \\sim C20 \\sim C19 \\sim C16 \\sim C15 \\sim C17: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C47 \\sim C46 \\sim C45 \\sim N3: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.01
O2 \\sim C55 \\sim O1: within 1.7A with sigma of 0.005 and sigma for terminal
atoms of 0.01
O2 \\sim C55 \\sim O1 \\sim C54 \\sim C53 \\sim C52 \\sim C50 \\sim C51: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C48 \\sim C49 \\sim N3 \\sim C47 \\sim C46 \\sim C45: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Co5 \\sim O15: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
O4 \\sim O15: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O15 \\sim O4 \\sim C33: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C33 \\sim O15: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.01
C33: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
O15 \\sim O4: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.01
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.001 and
sigma for terminal atoms of 0.002
Co5: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Co1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O18) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O18) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
Uanis(O15) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O9) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C26) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C26) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(O5) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Co5) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C46) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C8)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O15) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C33) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6.a Aromatic/amide H refined with riding coordinates:
 C35(H35), C42(H42), C53(H53), C51(H51), C43(H43), C29(H29), C30(H30),
 C37(H37), C7(H7), C6(H6), C4(H4), C3(H3), C13(H13), C28(H28), C32(H32), C9(H9),
  C34(H34), C36(H36), C52(H52), C50(H50), C11(H11), C22(H22), C23(H23),
 C25(H25), C26(H26), C19(H19), C20(H20), C15(H15), C16(H16), C48(H48), C46(H46),
  C47(H47), C49(H49)
6.b Fitted hexagon refined as free rotating group:
 C2(C7,C6,C5,C4,C3), C22(C23,C24,C25,C26,C21), C17(C19,C20,C14,C15,C16),
 C48(C45,C46,C47,N3,C49)
;
_shelx_res_checksum              59631
_shelx_hkl_checksum              89828
_shelx_fab_checksum              84695
_olex2_date_sample_data_collection 2018-05-10
_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 3.924
_oxdiff_exptl_absorpt_empirical_full_min 0.366