A window-space-directed assembly strategy for the construction of supertetrahedron-based zeolitic mesoporous metal-organic frameworks with ultramicroporous apertures for selective gas adsorption.
Zhang, Lei; Li, Fangfang; You, Jianjun; Hua, Nengbin; Wang, Qianting; Si, Junhui; Chen, Wenzhe; Wang, Wenjing; Wu, Xiaoyuan; Yang, Wenbin; Yuan, Daqiang; Lu, Canzhong; Liu, Yanrong; Al-Enizi, Abdullah M; Nafady, Ayman; Ma, Shengqian; Chemical science 12 (2021) 5767–5773; doi:10.1039/d0sc06841a

data_1560859
_publ_section_title
;
 A window-space-directed assembly strategy for the construction of
 supertetrahedron-based zeolitic mesoporous metal-organic frameworks with
 ultramicroporous apertures for selective gas adsorption.
;
_journal_issue                   16
_journal_name_full               'Chemical science'
_journal_page_first              5767
_journal_page_last               5773
_journal_paper_doi               10.1039/d0sc06841a
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         '0.04(C720 H425 Ni72 N96 O336)'
_chemical_formula_sum            'C30 H17 N4 Ni3 O14'
_chemical_formula_weight         747.10
_chemical_name_systematic        ST-sod-Ni
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-02 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   32.97540(10)
_cell_length_b                   32.97540(10)
_cell_length_c                   32.97540(10)
_cell_measurement_reflns_used    43086
_cell_measurement_temperature    104.5(7)
_cell_measurement_theta_max      60.5230
_cell_measurement_theta_min      2.8330
_cell_volume                     35856.69(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      104.5(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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     35.00  60.00   0.50    8.00    --   72.03-112.00 100.00   50
  2  \w     -2.00  24.00   0.50    8.00    --   72.03 -19.00  60.00   52
  3  \w     -1.00  26.00   0.50    8.00    --   72.03 -19.00  90.00   54
  4  \w    -16.00  41.00   0.50    2.00    --   -1.72  38.00 150.00  114
  5  \w    -33.00  -7.00   0.50    8.00    --  -75.46  38.00  30.00   52
  6  \w    -25.00   0.00   0.50    8.00    --  -75.46  19.00-120.00   50
  7  \w    -26.00  -1.00   0.50    8.00    --  -75.46  19.00-150.00   50
  8  \w    -26.00  -1.00   0.50    8.00    --  -75.46  19.00-180.00   50
  9  \w    -43.00  -2.00   0.50    8.00    --  -75.46  38.00-120.00   82
 10  \w    -42.00 -13.00   0.50    8.00    --  -75.46  38.00-150.00   58
 11  \w     -2.00  30.00   0.50    2.00    --   -1.72  38.00-150.00   64
 12  \w     37.00  71.00   0.50    2.00    --   -1.72  38.00-150.00   68
 13  \w     96.00 145.00   0.50    8.00    --   72.03 112.00-166.00   98
 14  \w     -3.00  22.00   0.50    8.00    --   72.03 -19.00 -60.00   50
 15  \w     -2.00  25.00   0.50    8.00    --   72.03 -19.00-120.00   54
 16  \w   -108.00 -54.00   0.50    8.00    --  -75.46 112.00-166.00  108
 17  \w   -117.00 -92.00   0.50    8.00    --  -75.46-112.00 100.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0335764000
_diffrn_orient_matrix_UB_12      -0.0187816000
_diffrn_orient_matrix_UB_13      0.0129314000
_diffrn_orient_matrix_UB_21      0.0214602000
_diffrn_orient_matrix_UB_22      -0.0181773000
_diffrn_orient_matrix_UB_23      0.0293290000
_diffrn_orient_matrix_UB_31      -0.0077767000
_diffrn_orient_matrix_UB_32      0.0310696000
_diffrn_orient_matrix_UB_33      0.0249770000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            100150
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.733
_diffrn_reflns_theta_min         2.854
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    5.431
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.830
_exptl_crystal_description       cube
_exptl_crystal_F_000             9010
_exptl_crystal_size_max          0.129
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.129
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         3885
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+174.2857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1774
_refine_ls_wR_factor_ref         0.1802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3646
_reflns_number_total             3885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06841a2.cif
_cod_data_source_block           ST-sod-Ni
_cod_depositor_comments
'Adding full bibliography for 1560858--1560860.cif.'
_cod_original_cell_volume        35856.7(3)
_cod_original_formula_sum        'C30 H17 Ni3 N4 O14'
_cod_database_code               1560859
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         NiCHNO
_shelx_estimated_absorpt_t_max   0.541
_shelx_estimated_absorpt_t_min   0.541
_diffrn_oxdiff_digest_frames
;
0180088aa3ac4c50e994dd0451399cfded0110434f5
;
_diffrn_oxdiff_digest_hkl
;
015f14e49ae9fa8b7239ca7733307608b1ccaf
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H2B-O2
 0.9 with sigma of 0.02
 H2A-O2
 0.9 with sigma of 0.02
3. Restrained planarity
 C0AA_$8, N0AB_$8, C0AA, N0AB, C0AA_$6, N0AB_$6
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C0AA) \\sim Ueq, Uanis(N0AB) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Sof(N0AB)=0.5*(1-FVAR(2))
 Sof(C0AA)=Sof(C1AA)=0.5*FVAR(2)
 Sof(C2AA)=Sof(H2AA)=Sof(C3AA)=Sof(H3AA)=FVAR(1)
 Fixed Sof: H2A(0.25) H2B(0.25)
6.a Rotating group:
 O2(H2A,H2B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C2AA(H2AA), C3AA(H3AA)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2663
_shelx_hkl_checksum              67834
_shelx_fab_checksum              70352
_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 4.032
_oxdiff_exptl_absorpt_empirical_full_min 0.523