A pacs-type metal–organic framework with high adsorption capacity for inverse C2H6/C2H4 separation
Zhang, Kuo; Pang, Jing-Jing; Lian, Xin; Song, Zi-Han; Yuan, Yue-Chao; Huang, Hongliang; Yao, Zhao-Quan; Xu, Jian; New Journal of Chemistry 48 (2024) 10577–10583; doi:10.1039/D4NJ00605D

data_7063226
_publ_section_title
;
 A pacs-type metal--organic framework with high adsorption capacity for
 inverse C2H6/C2H4 separation
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10577
_journal_page_last               10583
_journal_paper_doi               10.1039/D4NJ00605D
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C30 H36 Ni3 O13, 2(C9 H6 N3)'
_chemical_formula_sum            'C48 H48 N6 Ni3 O13'
_chemical_formula_weight         1093.05
_chemical_name_common            Ni-bodc-tpt
_chemical_name_systematic        Ni-bodc-tpt
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-17
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-29 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.7926(6)
_cell_length_b                   16.7926(6)
_cell_length_c                   14.6396(9)
_cell_measurement_reflns_used    6767
_cell_measurement_temperature    210(90)
_cell_measurement_theta_max      75.5850
_cell_measurement_theta_min      4.2940
_cell_volume                     3575.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      210(90)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.949
_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     -3.00  22.00   0.50    5.00    --    0.00  13.00 145.00   50
  2  \w    -45.00 -20.00   0.50    5.00    --    0.00 -13.00 -25.00   50
  3  \w     65.00  91.00   0.50   20.00    --  101.30 -13.00 -25.00   52
  4  \w    138.00 164.00   0.50   20.00    --  101.30  13.00 145.00   52
  5  \w    -35.00  23.00   0.50    5.00    --    0.00 -82.00 -30.00  116
  6  \w    -23.00  37.00   0.50    5.00    --    0.00  82.00 -90.00  120
  7  \w     -5.00  20.00   0.50    5.00    --    0.00  82.00-180.00   50
  8  \w     78.00 160.00   0.50   20.00    --  101.30  38.00-180.00  164
  9  \w     51.00 112.00   0.50   20.00    --  101.30 -77.00-150.00  122
 10  \w     52.00 123.00   0.50   20.00    --  101.30 -38.00 -60.00  142
 11  \w     17.00 117.00   0.50   20.00    --  101.30 -57.00-150.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0092904000
_diffrn_orient_matrix_UB_12      0.0416952000
_diffrn_orient_matrix_UB_13      -0.0903838000
_diffrn_orient_matrix_UB_21      -0.0154354000
_diffrn_orient_matrix_UB_22      0.0699449000
_diffrn_orient_matrix_UB_23      0.0539367000
_diffrn_orient_matrix_UB_31      0.1043652000
_diffrn_orient_matrix_UB_32      0.0677130000
_diffrn_orient_matrix_UB_33      -0.0000204000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12516
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.057
_diffrn_reflns_theta_min         4.285
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.015
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dimethylacetamide?DI water'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         1417
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0689
_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^)+(0.1233P)^2^+3.2310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2075
_refine_ls_wR_factor_ref         0.2255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1198
_reflns_number_total             1417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj00605d2.cif
_cod_data_source_block           ni-tpt
_cod_depositor_comments
'Adding full bibliography for 7063225--7063226.cif.'
_cod_database_code               7063226
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Ni'
_chemical_oxdiff_usercomment     'C H O N Ni'
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.778
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O4-C10 = O3-C10 = O2-C1 = O1-C1
 1.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4 \\sim C10 \\sim C9 \\sim C8 \\sim C5 \\sim C6 \\sim C4 \\sim C3 \\sim C7
\\sim O3 \\sim C1 \\sim O2 \\sim O1 \\sim C2: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
Uanis(O4) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C1) \\sim Ueq,
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: O4(0.333333) C10(0.333333) C9(0.333333) C8(0.333333) H8A(0.333333)
 H8B(0.333333) C5(0.166667) H5A(0.166667) H5B(0.166667) C6(0.333333)
 H6A(0.333333) H6B(0.333333) C4(0.333333) H4A(0.333333) H4B(0.333333)
 C3(0.166667) H3A(0.166667) H3B(0.166667) C7(0.166667) H7A(0.166667)
 H7B(0.166667) O3(0.333333) C1(0.166667) O2(0.166667) O1(0.166667) C2(0.166667)
 Fixed X: C9(0.4603) C5(0.54023) C2(0.544439)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C5(H5A,H5B), C6(H6A,H6B), C4(H4A,H4B), C3(H3A,H3B), C7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68424
_shelx_hkl_checksum              19411
_shelx_fab_checksum              76454
_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 3.255
_oxdiff_exptl_absorpt_empirical_full_min 0.228