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_4134924
_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         'C57 H33 Co4.5 N4 O17.5'
_chemical_formula_sum            'C57 H33 Co4.5 N4 O17.5'
_chemical_formula_weight         1319.06
_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                   21.9069(4)
_cell_length_b                   21.9069(4)
_cell_length_c                   39.6456(13)
_cell_measurement_reflns_used    14299
_cell_measurement_temperature    293.26(16)
_cell_measurement_theta_max      28.1240
_cell_measurement_theta_min      3.6920
_cell_volume                     19026.4(8)
_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      293.26(16)
_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    -64.00  35.00   0.30   98.03    --   10.21 -38.00 150.00  330
  2  \w    -35.00  -9.80   0.30   98.03    --   10.21 -19.00-120.00   84
;
_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      -0.0021637000
_diffrn_orient_matrix_UB_12      0.0117750000
_diffrn_orient_matrix_UB_13      -0.0166500000
_diffrn_orient_matrix_UB_21      0.0295707000
_diffrn_orient_matrix_UB_22      0.0128024000
_diffrn_orient_matrix_UB_23      0.0015807000
_diffrn_orient_matrix_UB_31      0.0129629000
_diffrn_orient_matrix_UB_32      -0.0272960000
_diffrn_orient_matrix_UB_33      -0.0064160000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0682
_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       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            59107
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.338
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41019
_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    0.921
_exptl_crystal_description       block
_exptl_crystal_F_000             5316
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;

;
_refine_diff_density_max         1.978
_refine_diff_density_min         -2.593
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Flack x determined using 4882 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.499(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         19224
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0922
_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^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2674
_refine_ls_wR_factor_ref         0.2939
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                13218
_reflns_number_total             19224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00612_si_002.cif
_cod_data_source_block           FJU-6-NDC
_cod_original_cell_volume        19026.3(10)
_cod_original_formula_sum        'C57 H33 Co4.50 N4 O17.50'
_cod_database_code               4134924
_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   0.984
_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
 C53-C53_$1
 2.78 with sigma of 0.02
 C54_$1-C54
 2.78 with sigma of 0.02
 C57-C57_$1
 2.78 with sigma of 0.02
 C57-C53
 1.4 with sigma of 0.02
 C54-C53
 1.4 with sigma of 0.02
 C54-C57_$1
 1.4 with sigma of 0.02
 C57_$1-C53_$1
 1.4 with sigma of 0.02
 C54_$1-C53_$1
 1.4 with sigma of 0.02
 C58-C55_$1
 2.78 with sigma of 0.02
 C56_$1-C57
 2.78 with sigma of 0.02
 C59-C54_$1
 2.78 with sigma of 0.02
 C58-C59
 1.4 with sigma of 0.02
 C56_$1-C59
 1.4 with sigma of 0.02
 C55_$1-C56_$1
 1.4 with sigma of 0.02
 C55_$1-C54_$1
 1.4 with sigma of 0.02
 C54_$1-C57
 1.4 with sigma of 0.02
 C58-C57
 1.4 with sigma of 0.02
 O14-C27
 1.23 with sigma of 0.02
 C57-C53 \\sim C54-C53 \\sim C54-C57_$1 \\sim C57_$1-C53_$1 \\sim C54_$1-C53_$1
\\sim C54_$1-C57
 with sigma of 0.02
 C58-C59 \\sim C58-C57 \\sim C56_$1-C59 \\sim C55_$1-C56_$1 \\sim C55_$1-C54_$1
\\sim C54_$1-C57
 with sigma of 0.02
3. Restrained planarity
 C57, C53, C54, C57_$1, C53_$1, C54_$1
 with sigma of 0.1
 C58, C59, C56_$1, C55_$1, C54_$1, C57
 with sigma of 0.1
4. Rigid bond restraints
 C42, C43, N48, C45, C44, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C56, C55, C54, C53, C57, C58, C59
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O14, C27, O13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C41 \\sim C44 \\sim C45 \\sim N48 \\sim C43 \\sim C42: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C58 \\sim C59 \\sim C57 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
O14 \\sim C27 \\sim O13: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(O19)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(N48) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Fixed Sof: C56(0.5) H56(0.5) C58(0.5) H58(0.5) C55(0.5) H55(0.5) C59(0.5)
 H59(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C37(H37), C47(H47), C46(H46), C5(H5), C6(H6), C4(H4), C3(H3), C32(H32),
 C29(H29), C31(H31), C34(H34), C35(H35), C19(H19), C49(H49), C11(H11), C28(H28),
  C42(H42), C43(H43), C45(H45), C44(H44), C9(H9), C13(H13), C16(H16), C22(H22),
 C23(H23), C25(H25), C24(H24), C18(H18), C48(H48), C36(H36), C15(H15), C56(H56),
  C58(H58), C55(H55), C59(H59)
7.b Fitted hexagon refined as free rotating group:
 C2(C5,C6,C7,C4,C3), C41(C42,C43,N48,C45,C44), C21(C22,C23,C26,C25,C24)
;
_shelx_res_checksum              94902
_shelx_hkl_checksum              76889
_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 1.461
_oxdiff_exptl_absorpt_empirical_full_min 0.513