Configurational control of low-symmetry heteroleptic metal-organic cages with asymmetric ligands.
Yu, Hao; Guo, Ziteng; Tang, Jie; Han, Ningxu; Shi, Junjuan; Li, Meng; Zhang, Houyu; Wang, Ming; Chemical science 16 (2025) 6114–6120; doi:10.1039/d4sc08647c

data_1574093
_publ_section_title
;
 Configurational control of low-symmetry heteroleptic metal-organic cages
 with asymmetric ligands.
;
_journal_issue                   14
_journal_name_full               'Chemical science'
_journal_page_first              6114
_journal_page_last               6120
_journal_paper_doi               10.1039/d4sc08647c
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C282 H204 N24 Pd6'
_chemical_formula_sum            'C282 H204 N24 Pd6'
_chemical_formula_weight         4567.08
_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-09
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2025-02-10 deposited with the CCDC.	2025-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   26.2350(17)
_cell_length_b                   26.2350(17)
_cell_length_c                   46.357(4)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      16.229
_cell_measurement_theta_min      2.272
_cell_volume                     27632(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Synchrotron radiation X-ray'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6887
_diffrn_reflns_av_R_equivalents  0.1274
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            99021
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        16.499
_diffrn_reflns_theta_max         16.499
_diffrn_reflns_theta_min         0.868
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.4068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1973 before and 0.0759 after correction.
The Ratio of minimum to maximum transmission is 0.5468.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.549
_exptl_crystal_description       block
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.397
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5238
_refine_ls_number_restraints     1204
_refine_ls_restrained_S_all      1.315
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.1258
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3361
_refine_ls_wR_factor_ref         0.3594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3969
_reflns_number_total             5238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08647c2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1574092--1574094.cif.'
_cod_original_cell_volume        27632(4)
_cod_database_code               1574093
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.970
_olex2_refinement_description
;
1. Restrained distances
 C45-C47
 1.5 with sigma of 0.01
 C11-C23
 1.5 with sigma of 0.01
 C23-C45
 1.2 with sigma of 0.01
 H15-H32
 2.2 with sigma of 0.01
 C31-C40
 1.5 with sigma of 0.01
 C40-C31
 1.45 with sigma of 0.01
 C7-C17
 1.5 with sigma of 0.01
2. Rigid bond restraints
 N4, Pd1, N2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C1 \\sim C4 \\sim C6 \\sim C8 \\sim C10 \\sim C7 \\sim C29 \\sim C15 \\sim C31
\\sim C2 \\sim C33 \\sim C17 \\sim C13 \\sim C35 \\sim C9 \\sim C19 \\sim C37
\\sim C12 \\sim C14 \\sim C16 \\sim C18 \\sim C20 \\sim C22 \\sim C24 \\sim C26
\\sim C28 \\sim C30 \\sim C23 \\sim C27 \\sim C32 \\sim C34 \\sim C36 \\sim C38
\\sim C40 \\sim C39 \\sim C5 \\sim C41 \\sim C21 \\sim C43 \\sim C11 \\sim C42
\\sim C44 \\sim C46 \\sim C47 \\sim C3 \\sim C25 \\sim C45 \\sim N1 \\sim N4
\\sim N2 \\sim N3: within 3.8A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 3.8A
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C10(H10), C29(H29), C15(H15), C2(H2), C33(H33),
 C13(H13), C9(H9), C19(H19), C37(H37), C12(H12), C14(H14), C18(H18), C20(H20),
 C24(H24), C26(H26), C28(H28), C30(H30), C32(H32), C36(H36), C38(H38), C39(H39),
  C5(H5), C21(H21), C43(H43), C44(H44), C46(H46), C3(H3), C25(H25)
4.b Fitted hexagon refined as free rotating group:
 N1(C1,C4,C6,C8,C10), C7(C29,C15,C31,C2,C33), C17(C13,C35,C9,C19,C37), C12(N4,
 C14,C16,C18,C20), C22(C24,C26,N2,C28,C30), C32(C34,N3,C36,C38,C40), C39(C5,C41,
 C21,C43,C11), C42(C44,C46,C47,C3,C25)
4.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              72723
_shelx_fab_checksum              75601
_olex2_submission_special_instructions 'No special instructions were received'