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_1568928
_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         'C94 H108 Al8 N24 O36'
_chemical_formula_sum            'C94 H100 Al8 N24 O38'
_chemical_formula_weight         2389.81
_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     iterative
_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                   36.6848(4)
_cell_length_b                   36.6848(4)
_cell_length_c                   36.6848(4)
_cell_measurement_reflns_used    17809
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.1860
_cell_measurement_theta_min      2.1650
_cell_volume                     49369.5(9)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_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 0.988
_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   -117.00 -88.00   0.50    7.04    --  -74.78 -99.00 -30.00   58
  2  \w   -148.00-121.00   0.50    7.04    --  -74.78 -99.00 -30.00   54
  3  \w    -13.00  14.00   0.50    1.76    --   -0.62 -78.00 -90.00   54
  4  \w     88.00 147.00   0.50    7.04    --   73.53 119.00  86.00  118
;
_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      -0.0114092000
_diffrn_orient_matrix_UB_12      0.0346671000
_diffrn_orient_matrix_UB_13      -0.0001697000
_diffrn_orient_matrix_UB_21      -0.0130259000
_diffrn_orient_matrix_UB_22      -0.0040952000
_diffrn_orient_matrix_UB_23      0.0338762000
_diffrn_orient_matrix_UB_31      0.0321578000
_diffrn_orient_matrix_UB_32      0.0106985000
_diffrn_orient_matrix_UB_33      0.0135628000
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            35760
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.605
_diffrn_reflns_theta_min         2.565
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11070
_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    0.965
_exptl_crystal_description       cube
_exptl_crystal_F_000             14880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 2946 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.346(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         9351
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0943P)^2^+9.6419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1468
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                8021
_reflns_number_total             9351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01260c6.cif
_cod_data_source_block           AlOC-58
_cod_depositor_comments
'Adding full bibliography for 1568928--1568931.cif.'
_cod_original_cell_volume        49369.5(16)
_cod_database_code               1568928
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Al Fe Cl C N O'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H4C,H4D} of C4, {H2C,H2D} of C2, {H5A,H5B} of C5, {H3A,
  H3B} of C3, All N(H,H) groups, All O(H) groups
 At 1.5 times of:
  {H6A,H6B} of C6, {H1A,H1B} of C1
2. Restrained distances
 C2-C1
 1.45 with sigma of 0.01
3. Rigid bond restraints
 C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O9, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.02
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5)
6.a Riding coordinates:
 O3(H3), C3(H3A,H3B), C4(H4C,H4D), C2(H2C,H2D), C5(H5A,H5B), C6(H6A,H6B),
 C1(H1A,H1B)
6.b Rotating group:
 N7(H7A,H7B)
6.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C18(H18), C15(H15), C17(H17), C24(H24), C23(H23), C9(H9), C12(H12),
 C11(H11)
6.d X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60982
_shelx_hkl_checksum              450
_shelx_fab_checksum              34411
_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 3.932
_oxdiff_exptl_absorpt_empirical_full_min 0.462