Two amino-functionalized metal-organic frameworks with different topologies for C<sub>2</sub>H<sub>2</sub>/C<sub>2</sub>H<sub>4</sub> separation.
Li, Yue; Xu, Mingming; Liu, Hongyan; Wang, Xiaokang; Wang, Yutong; Sun, Meng; Fan, Weidong; Sun, Daofeng; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18094–18098; doi:10.1039/d4dt02592j

data_7717425
_publ_section_title
;
 Two amino-functionalized metal-organic frameworks with different
 topologies for C<sub>2</sub>H<sub>2</sub>/C<sub>2</sub>H<sub>4</sub>
 separation.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18094
_journal_page_last               18098
_journal_paper_doi               10.1039/d4dt02592j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C38 H33 N4 Ni3 O13'
_chemical_formula_sum            'C38 H33 N4 Ni3 O13'
_chemical_formula_weight         929.81
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-08-12 deposited with the CCDC.	2024-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   23.5121(12)
_cell_length_b                   23.5121(12)
_cell_length_c                   38.3738(12)
_cell_measurement_reflns_used    2864
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      57.1980
_cell_measurement_theta_min      4.4790
_cell_volume                     18371.7(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.976
_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    -61.00  -6.00   1.00   35.00    --    0.00 130.00 -85.00   55
  2  \w    -24.00  33.00   1.00   35.00    --    0.00 -80.00 145.00   57
  3  \w    -15.00  75.00   1.00   35.00    --   53.63 -57.00-150.00   90
  4  \w     32.00 102.00   1.00   35.00    --   53.63-140.00  28.00   70
  5  \w     26.00 109.00   1.00   35.00    --   53.63-125.00-180.00   83
  6  \w    111.00 176.00   1.00   40.00    --  107.26 111.00 120.00   65
  7  \w     85.00 159.00   1.00   40.00    --  107.26  63.00-120.00   74
  8  \w    100.00 177.00   1.00   40.00    --  107.26  80.00 -90.00   77
  9  \w    121.00 162.00   1.00   40.00    --  107.26 111.00-120.00   41
 10  \w     52.00  87.00   1.00   40.00    --  107.26 -50.00 150.00   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0155281000
_diffrn_orient_matrix_UB_12      0.0402973000
_diffrn_orient_matrix_UB_13      0.0260628000
_diffrn_orient_matrix_UB_21      0.0567202000
_diffrn_orient_matrix_UB_22      0.0639845000
_diffrn_orient_matrix_UB_23      -0.0151350000
_diffrn_orient_matrix_UB_31      -0.0475773000
_diffrn_orient_matrix_UB_32      0.0029064000
_diffrn_orient_matrix_UB_33      -0.0265497000
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            15185
_diffrn_reflns_point_group_measured_fraction_full 0.611
_diffrn_reflns_point_group_measured_fraction_max 0.594
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.616
_diffrn_reflns_theta_min         3.760
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.756
_exptl_crystal_description       block
_exptl_crystal_F_000             4293
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         9324
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0970P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1850
_reflns_Friedel_coverage         0.217
_reflns_Friedel_fraction_full    0.225
_reflns_Friedel_fraction_max     0.212
_reflns_number_gt                5493
_reflns_number_total             9324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02592j2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7717425--7717426.cif.'
_cod_original_cell_volume        18371.7(19)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7717425
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Ni'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(5)
 0.48(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Riding coordinates:
 O1(H1), O4(H4A,H4B), O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C12(H12), C14(H14), C15(H15),
 C17(H17), C18(H18), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C31(H31),
  C33(H33), C34(H34), C36(H36), C37(H37)
5.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N10(H10A,H10B)
;
_shelx_res_checksum              92260
_shelx_hkl_checksum              13674
_shelx_fab_checksum              95670
_platon_squeeze_void_probe_radius 1.20
_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 1.468
_oxdiff_exptl_absorpt_empirical_full_min 0.682