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_1568930
_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, 4(C7 H5 O)'
_chemical_formula_sum            'C124 H100 Al8 N32 O44'
_chemical_formula_weight         2958.19
_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
_atom_sites_solution_primary     dual
_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                   22.8500(3)
_cell_length_b                   22.8500(3)
_cell_length_c                   14.9095(4)
_cell_measurement_reflns_used    6742
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      70.0630
_cell_measurement_theta_min      2.7190
_cell_volume                     7784.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.972
_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     62.00 164.00   0.50    1.28    --  105.36 152.00 -18.00  204
  2  \w     25.00  81.00   0.50    0.32    --   47.08  77.00  60.00  112
  3  \w    -26.00  47.00   0.50    0.32    --   47.08 -38.00  60.00  146
  4  \w     33.00 111.00   0.50    1.28    --  105.36-125.00  90.00  156
  5  \w     33.00  75.00   0.50    1.28    --  105.36 -61.00  60.00   84
  6  \w    -27.00  30.00   0.50    0.32    --   47.08 -19.00  90.00  114
  7  \w   -174.00 -89.00   0.50    1.28    -- -104.50 -12.00-176.00  170
  8  \w   -174.00 -92.00   0.50    1.28    -- -104.50 -30.00-180.00  164
  9  \w   -119.00 -53.00   0.50    0.32    --  -47.08-156.00-149.00  132
 10  \w   -101.00 -32.00   0.50    1.28    -- -104.50  77.00  60.00  138
 11  \w    -68.00 -32.00   0.50    1.28    -- -104.50  61.00-150.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0438282000
_diffrn_orient_matrix_UB_12      0.0512784000
_diffrn_orient_matrix_UB_13      -0.0003569000
_diffrn_orient_matrix_UB_21      0.0506050000
_diffrn_orient_matrix_UB_22      -0.0432265000
_diffrn_orient_matrix_UB_23      -0.0164035000
_diffrn_orient_matrix_UB_31      -0.0082796000
_diffrn_orient_matrix_UB_32      0.0068121000
_diffrn_orient_matrix_UB_33      -0.1019705000
_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  0.0369
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19245
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.667
_diffrn_reflns_theta_min         3.540
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
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    1.262
_exptl_crystal_description       plate
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 1234 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.12(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3983
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0967
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2670
_refine_ls_wR_factor_ref         0.2804
_reflns_Friedel_coverage         0.755
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                3417
_reflns_number_total             3983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01260c6.cif
_cod_data_source_block           4Bz@AlOC-59
_cod_depositor_comments
'Adding full bibliography for 1568928--1568931.cif.'
_cod_database_code               1568930
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Al C N O'
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.639
_olex2_refinement_description
;
1. Restrained distances
 H1A_$1-H1A
 2.2 with sigma of 0.02
 H00R_$2-H1B
 2.2 with sigma of 0.02
 H1B-H00R_$2
 2.2 with sigma of 0.02
2. Rigid bond restraints
 C00N, C00P, C00S, C00E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N00H
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C00E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N00O, C00M
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C00R, C00K
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C00F
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C00N) \\sim Ueq, Uanis(C00S) \\sim Ueq, Uanis(C00P) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N00O) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C00R) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O3(0.5)
5.a Riding coordinates:
 O03(H03)
5.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00J(H00J), C00F(H00F), C00M(H00M), C00K(H00K), C00R(H00R),
 C00P(H00P), C00S(H00S), C47(H47)
5.c Fitted hexagon refined as free rotating group:
 N00O(C00M,C00I,C00E,C00K,C00R)
5.d X=CH2 refined with riding coordinates:
 N00H(H00A,H00C), N1(H1A,H1B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2082
_shelx_hkl_checksum              29499
_shelx_fab_checksum              77001
_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 1.609
_oxdiff_exptl_absorpt_empirical_full_min 0.563