Accurate binding of porous aluminum molecular ring catalysts with the substrate.
Luo, Dan; Xiao, Han; Zhang, Min-Yi; Li, Shang-Da; He, Liang; Lv, Hong; Li, Chun-Sen; Lin, Qi-Pu; Fang, Wei-Hui; Zhang, Jian; Chemical science 14 (2023) 5396–5404; doi:10.1039/d3sc01260c

data_1568929
_publ_section_title
;
 Accurate binding of porous aluminum molecular ring catalysts with the
 substrate.
;
_journal_issue                   20
_journal_name_full               'Chemical science'
_journal_page_first              5396
_journal_page_last               5404
_journal_paper_doi               10.1039/d3sc01260c
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C96 H88 Al8 N32 O40'
_chemical_formula_sum            'C96 H80 Al8 N32 O40'
_chemical_formula_weight         2537.76
_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_Hall           'I 4 2'
_space_group_name_H-M_alt        'I 4 2 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-10-23
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-10-24 deposited with the CCDC.	2023-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.0719(3)
_cell_length_b                   23.0719(3)
_cell_length_c                   14.7983(4)
_cell_measurement_reflns_used    5615
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      59.8830
_cell_measurement_theta_min      4.5310
_cell_volume                     7877.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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      9.00  38.00   0.50    0.34    --   -0.94  85.00   0.00   58
  2  \w    -14.00  18.00   0.50    0.34    --   -0.94  38.00 -90.00   64
  3  \w     37.00  62.00   0.50    0.34    --   -0.94  38.00 -90.00   50
  4  \w     79.00 136.00   0.50    1.35    --   73.43 125.00 -30.00  114
  5  \w     72.00 146.00   0.50    1.35    --   73.43 146.00  54.00  148
  6  \w    -70.00  -1.00   0.50    1.35    --  -75.30  36.00-171.00  138
  7  \w   -146.00-120.00   0.50    1.35    --  -75.30 -99.00 150.00   52
  8  \w   -135.00 -81.00   0.50    1.35    --  -75.30-125.00-150.00  108
;
_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      0.0266542000
_diffrn_orient_matrix_UB_12      0.0506813000
_diffrn_orient_matrix_UB_13      0.0149069000
_diffrn_orient_matrix_UB_21      -0.0440977000
_diffrn_orient_matrix_UB_22      0.0279177000
_diffrn_orient_matrix_UB_23      -0.0394439000
_diffrn_orient_matrix_UB_31      -0.0267075000
_diffrn_orient_matrix_UB_32      0.0043264000
_diffrn_orient_matrix_UB_33      0.0801237000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14401
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.635
_diffrn_reflns_theta_min         2.355
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 1260 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.12(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         4441
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0707
_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^)+(0.1708P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2046
_refine_ls_wR_factor_ref         0.2193
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                3510
_reflns_number_total             4441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01260c6.cif
_cod_data_source_block           AlOC-59
_cod_depositor_comments
'Adding full bibliography for 1568928--1568931.cif.'
_cod_database_code               1568929
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Al Fe C N O'
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.869
_olex2_refinement_description
;
1. Rigid bond restraints
 N00M, N00E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C00C, C00G
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C00K, C00H
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C00O, C00H
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C00G, C00C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(N00M) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00K) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00O) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00J) \\sim Ueq, Uanis(C00F) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C00C) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Riding coordinates:
 O04(H04)
3.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00G(H00G), C00I(H00I), C00K(H00K), C00O(H00O), C00J(H00J)
3.c Fitted hexagon refined as free rotating group:
 C00K(N00M,C00O,C00J,C00F,C00H)
3.d X=CH2 refined with riding coordinates:
 N00E(H00A,H00B), N00N(H00C,H00E)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38724
_shelx_hkl_checksum              79151
_shelx_fab_checksum              26736
_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 1.234
_oxdiff_exptl_absorpt_empirical_full_min 0.515