Spatial disposition of square-planar mononuclear nodes in metal-organic frameworks for C<sub>2</sub>H<sub>2</sub>/CO<sub>2</sub> separation.
Zeng, Heng; Xie, Xiao-Jing; Wang, Ying; Luo, Dong; Wei, Rong-Jia; Lu, Weigang; Li, Dan; Chemical science 13 (2022) 12876–12882; doi:10.1039/d2sc04324f

data_1567794
_publ_section_title
;
 Spatial disposition of square-planar mononuclear nodes in metal-organic
 frameworks for C<sub>2</sub>H<sub>2</sub>/CO<sub>2</sub> separation.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              12876
_journal_page_last               12882
_journal_paper_doi               10.1039/d2sc04324f
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety
'C16 H10 Cu N4 O4, 3(H2 O), 2(C2 H3 N), C1.5 H3 N0.75'
_chemical_formula_sum            'C21.5 H25 Cu N6.75 O7'
_chemical_formula_weight         553.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2bjndy
_audit_creation_date             2022-03-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-22 deposited with the CCDC.	2022-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.1530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.23210(10)
_cell_length_b                   13.23780(10)
_cell_length_c                   14.6287(2)
_cell_measurement_reflns_used    8535
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      76.5990
_cell_measurement_theta_min      3.0870
_cell_volume                     2751.90(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.946
_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    -39.00  24.00   0.50    0.50    --   -0.90 -82.00 150.00  126
  2  \w     13.00  88.00   0.50    0.50    --    0.90  38.00 -30.00  150
  3  \w    -13.00  15.00   0.50    0.50    --    0.90  82.00 150.00   56
  4  \w    -21.00   5.00   0.50    0.50    --    0.90  38.00 -30.00   52
  5  \w     89.00 115.00   0.50    1.08    --  105.10  19.00-120.00   52
  6  \w    166.00 192.00   0.50    1.08    --  105.10  19.00-120.00   52
  7  \w     93.00 187.00   0.50    1.08    --  105.10  38.00  30.00  188
  8  \w     86.00 133.00   0.50    1.08    --  105.10 -82.00-120.00   94
  9  \w     20.00 140.00   0.50    1.08    --  105.10 -82.00-150.00  240
 10  \w     30.00 138.00   0.50    1.08    --  105.10 -77.00  60.00  216
 11  \w     82.00 141.00   0.50    1.08    --  105.10  82.00 -30.00  118
 12  \w    123.00 184.00   0.50    1.08    --  105.10  38.00  60.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14174
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.553
_diffrn_reflns_theta_min         4.565
_exptl_absorpt_coefficient_mu    1.557
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             1145
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.651
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.0036(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5536
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.1134
_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^)+(0.1441P)^2^+14.9399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2897
_refine_ls_wR_factor_ref         0.2960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4900
_reflns_number_total             5536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04324f2.cif
_cod_data_source_block           jnu-4
_cod_depositor_comments          'Adding full bibliography for 1567794.cif.'
_cod_original_formula_sum        'C21.50 H25 Cu N6.75 O7'
_cod_database_code               1567794
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.860
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C17-N5
 1.137 with sigma of 0.01
 C17-C18
 1.456 with sigma of 0.01
 C18-N5
 2.593 with sigma of 0.02
 C19-N6
 1.137 with sigma of 0.01
 C19-C20
 1.456 with sigma of 0.01
 C20-N6
 2.593 with sigma of 0.02
 C21-N7
 1.137 with sigma of 0.01
 C21-C22
 1.456 with sigma of 0.01
 C22-N7
 2.593 with sigma of 0.02
 C23-N8
 1.137 with sigma of 0.01
 C23-C24
 1.456 with sigma of 0.01
 C24-N8
 2.593 with sigma of 0.02
 N8-O4
 3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N5 \\sim C17 \\sim C18: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N6 \\sim C19 \\sim C20: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N7 \\sim C21 \\sim C22: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N8 \\sim C23 \\sim C24: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 N6, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C17, C18
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 C20, N6, C19
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 N7, C21, C22
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 N8, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N5(0.5) C17(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) N6(0.75)
 C19(0.75) C20(0.75) N8(0.5) C23(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
6.a Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B), N5(C17,C18), N6(C19,C20), N7(C21,C22),
 N8(C23,C24)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16)
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              42552
_shelx_hkl_checksum              80029
_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
;