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_4134920
_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         'C54 H32 Co4.5 N5 O17.5'
_chemical_formula_sum            'C54 H32 Co4.5 N5 O17.5'
_chemical_formula_weight         1296.03
_chemical_name_systematic        b
_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             2018-12-25
_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                   21.81320(10)
_cell_length_b                   21.81320(10)
_cell_length_c                   39.0403(9)
_cell_measurement_reflns_used    21625
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.1170
_cell_measurement_theta_min      3.4930
_cell_volume                     18576.0(4)
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_number            75233
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.342
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_type   none
_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    0.927
_exptl_crystal_description       block
_exptl_crystal_F_000             5220
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;

;
_refine_diff_density_max         1.852
_refine_diff_density_min         -1.957
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Flack x determined using 5792 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.493(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         18871
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      7.170
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0736
_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^)+(0.1520P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2146
_refine_ls_wR_factor_ref         0.2293
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                14465
_reflns_number_total             18871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00612_si_002.cif
_cod_data_source_block           FJU-6-PTB
_cod_original_cell_volume        18576.0(5)
_cod_original_formula_sum        'C54 H32 Co4.50 N5 O17.50'
_cod_database_code               4134920
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.851
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O13_$2-C19_$2
 1.2 with sigma of 0.02
 O13-C19
 1.15 with sigma of 0.02
 Co5_$1-O13_$2
 1.9 with sigma of 0.02
3. Rigid bond restraints
 C28, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C28, C27, C32, C31, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C46, C45, C44, C43, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33, C34, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C10, C9, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C28 \\sim C9: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C28 \\sim C9 \\sim C30 \\sim C34 \\sim C43: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C43 \\sim C44 \\sim C45 \\sim C46 \\sim N4 \\sim C42: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
C32 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C34 \\sim C43 \\sim C42 \\sim N4 \\sim C46 \\sim C45 \\sim C44: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C34 \\sim C33 \\sim C35: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
C9 \\sim C10 \\sim C8: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\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(C25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C53) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O8) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.0002
Uanis(C54) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C41) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C38) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C42) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O18) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C49) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C50) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C51) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C45) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C45) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C37) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C40) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C32) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C45(H45), C33(H33), C46(H46), C34(H34), C22(H22), C30(H30), C36(H36), C9(H9),
 C23(H23), C21(H21), C31(H31), C27(H27), C2(H2), C52(H52), C51(H51), C50(H50),
 C49(H49), C20(H20), C42(H42), C43(H43), C37(H37), C4(H4), C28(H28), C3(H3),
 C6(H6), C7(H7), C40(H40), C41(H41), C18(H18), C17(H17), C15(H15), C14(H14)
5.b Fitted hexagon refined as free rotating group:
 C52(C51,N3,C50,C49,C48), C18(C17,C16,C15,C14,C13)
;
_shelx_res_checksum              6629
_shelx_hkl_checksum              51051
_olex2_submission_special_instructions 'No special instructions were received'