Cooperative reversible assembly in triply interlocked Al<sub>6</sub>L<sub>4</sub> and Ga<sub>6</sub>L<sub>4</sub> cages.
Izquierdo, Ignacio; Martínez-Castro, Laura; Ujaque, Gregori; Martínez-Martínez, Antonio J; Chemical science 16 (2025) 20406–20413; doi:10.1039/d5sc05441a

data_1575870
_publ_section_title
;
 Cooperative reversible assembly in triply interlocked
 Al<sub>6</sub>L<sub>4</sub> and Ga<sub>6</sub>L<sub>4</sub> cages.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              20406
_journal_page_last               20413
_journal_paper_doi               10.1039/d5sc05441a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C36 H33 N9 O6'
_chemical_formula_sum            'C36 H33 N9 O6'
_chemical_formula_weight         687.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2025-09-01 deposited with the CCDC.	2025-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3821(2)
_cell_length_b                   27.7393(5)
_cell_length_c                   11.5669(2)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.465
_cell_measurement_theta_min      2.324
_cell_volume                     3257.78(10)
_computing_cell_refinement       'Bruker Apex3, 2020'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            198296
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.528
_diffrn_reflns_theta_min         2.323
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.1418
_exptl_absorpt_correction_T_min  0.1102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0989 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.7772.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         9960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0706P)^2^+1.9568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8940
_reflns_number_total             9960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05441a2.cif
_cod_data_source_block           081am21nippstris100k_0m
_cod_depositor_comments
'Adding full bibliography for 1575870--1575871.cif.'
_cod_database_code               1575870
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.975
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C8(H8), C12(H12), C13(H13), C14(H14), C18(H18),
 C22(H22), C23(H23), C24(H24), C28(H28), C32(H32), C33(H33), C34(H34)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              63714
_olex2_submission_special_instructions 'No special instructions were received'