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_1568931
_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         'C88 H96 Al8 N24 O36'
_chemical_formula_sum            'C88 H88 Al8 N24 O36'
_chemical_formula_weight         2273.66
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_Hall           'I 4 2 3'
_space_group_name_H-M_alt        'I 4 3 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            12
_cell_length_a                   36.6170(3)
_cell_length_b                   36.6170(3)
_cell_length_c                   36.6170(3)
_cell_measurement_reflns_used    32054
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.7350
_cell_measurement_theta_min      2.3430
_cell_volume                     49096.2(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_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 0.981
_diffrn_measured_fraction_theta_max 0.977
_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   -101.00 -32.00   0.50    1.98    -- -104.50  77.00 -60.00  138
  2  \w    -68.00 -32.00   0.50    1.98    -- -104.50  61.00 120.00   72
  3  \w   -119.00 -74.00   0.50    0.50    --  -47.08-125.00 120.00   90
  4  \w   -101.00 -32.00   0.50    1.98    -- -104.50  77.00 -90.00  138
  5  \w    -82.00   7.00   0.50    0.50    --  -47.08 103.00 -84.00  178
  6  \w     25.00 120.00   0.50    0.50    --   47.08  77.00 -60.00  190
  7  \w     32.00 120.00   0.50    0.50    --   47.08  57.00-150.00  176
  8  \w     35.00  98.00   0.50    0.50    --   47.08  38.00  60.00  126
  9  \w     93.00 178.00   0.50    1.98    --  105.36  30.00  90.00  170
 10  \w    -27.00  30.00   0.50    0.50    --   47.08 -19.00 -90.00  114
 11  \w     33.00 123.00   0.50    1.98    --  105.36-141.00-166.00  180
 12  \w     33.00 108.00   0.50    1.98    --  105.36 -77.00  30.00  150
 13  \w     33.00  75.00   0.50    1.98    --  105.36 -61.00 120.00   84
 14  \w     33.00  90.00   0.50    1.98    --  105.36 -70.00 161.00  114
;
_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      -0.0052693475
_diffrn_orient_matrix_UB_12      0.0416621475
_diffrn_orient_matrix_UB_13      -0.0027102525
_diffrn_orient_matrix_UB_21      0.0324984974
_diffrn_orient_matrix_UB_22      0.0058012026
_diffrn_orient_matrix_UB_23      0.0260676026
_diffrn_orient_matrix_UB_31      0.0261606504
_diffrn_orient_matrix_UB_32      0.0011725496
_diffrn_orient_matrix_UB_33      -0.0329646504
_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  0.0719
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            155022
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.007
_diffrn_reflns_theta_min         2.956
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.54a (Rigaku Oxford Diffraction, 2022)
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    0.923
_exptl_crystal_description       plate
_exptl_crystal_F_000             14112
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 3089 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.043(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         8511
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0521
_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^)+(0.1068P)^2^+4.7268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                7725
_reflns_number_total             8511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01260c6.cif
_cod_data_source_block           Bz@AlOC-58
_cod_depositor_comments
'Adding full bibliography for 1568928--1568931.cif.'
_cod_original_cell_volume        49096.2(12)
_cod_database_code               1568931
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Al C N O'
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.754
_olex2_refinement_description
;
1. Rigid bond restraints
 C00Z
 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(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00Z) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C46) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: C00Z(0.5) H00Z(0.5) C2(0.5) H2(0.5) C6(0.5) H6(0.5) C46(0.5)
 H46(0.5)
4.a Riding coordinates:
 O06(H06), C012(H01C,H01D), C11(H11A,H11B)
4.b Secondary CH2 refined with riding coordinates:
 C010(H01A,H01B), C015(H01E,H01F)
4.c Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00P(H00P), C00Q(H00Q), C00R(H00R), C00T(H00T), C00V(H00V),
 C00Z(H00Z), C5(H5), C2(H2), C6(H6), C46(H46)
4.d X=CH2 refined with riding coordinates:
 N00F(H00A,H00B), N00L(H00C,H00D), N00U(H00E,H00F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96611
_shelx_hkl_checksum              53398
_shelx_fab_checksum              54772
_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 1.376
_oxdiff_exptl_absorpt_empirical_full_min 0.781