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_1574094
_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         '0.333(C528 H384 N48 Pd12), 0.167[]'
_chemical_formula_sum            'C176 H128 N16 Pd4'
_chemical_formula_weight         2892.54
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_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                90
_cell_formula_units_Z            6
_cell_length_a                   43.650(2)
_cell_length_b                   43.650(2)
_cell_length_c                   43.650(2)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      12.915
_cell_measurement_theta_min      2.213
_cell_volume                     83167(7)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68874
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0084
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            105940
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        14.239
_diffrn_reflns_theta_max         14.239
_diffrn_reflns_theta_min         1.430
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.7438
_exptl_absorpt_correction_T_min  0.6587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0688 before and 0.0566 after correction.
The Ratio of minimum to maximum transmission is 0.8856.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.347
_exptl_crystal_description       block
_exptl_crystal_F_000             8880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.582
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         1484
_refine_ls_number_restraints     811
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.1934
_refine_ls_R_factor_gt           0.1841
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.4500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5160
_refine_ls_wR_factor_ref         0.5750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1290
_reflns_number_total             1484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08647c2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 1574092--1574094.cif.'
_cod_original_cell_volume        83166(12)
_cod_database_code               1574094
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.974
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C00P-C00D
 1.45 with sigma of 0.01
 C00D-C00P
 1.45 with sigma of 0.01
 C11-C7
 1.45 with sigma of 0.01
 C9-C1
 1.45 with sigma of 0.01
3. Restrained planarity
 C005, N003, C3, C006, C00D, C00C, C00P, C00G, C007, C1, C00N, C00U, C00B, C10,
  N2, C4, C5, C11, C6, C12, C13, C9, C8, C7
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C005 \\sim C3 \\sim C006 \\sim C00D \\sim C00C \\sim C00P \\sim C00G \\sim C007
\\sim C1 \\sim C00N \\sim C00U \\sim C00B \\sim C10 \\sim C4 \\sim C5 \\sim C11
\\sim C6 \\sim C12 \\sim C13 \\sim C9 \\sim C8 \\sim C7 \\sim N003 \\sim N2:
within 5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 5A
5. Others
 Fixed Sof: C005(0.5) H005(0.5) N003(0.5) C3(0.5) H3(0.5) C006(0.5) H006(0.5)
 C00D(0.5) C00C(0.5) H00C(0.5) C00P(0.5) C00G(0.5) H00G(0.5) C007(0.5)
 H007(0.5) C1(0.5) C00N(0.5) H00N(0.5) C00U(0.5) H00U(0.5) C00B(0.5) H00B(0.5)
 C10(0.5) H10(0.5) N2(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5) C11(0.5) C6(0.5)
 H6(0.5) C12(0.5) H12(0.5) C13(0.5) H13(0.5) C9(0.5) C8(0.5) H8(0.5) C7(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C005(H005), C3(H3), C006(H006), C00C(H00C), C00G(H00G), C007(H007),
 C00N(H00N), C00U(H00U), C00B(H00B), C10(H10), C4(H4), C5(H5), C6(H6), C12(H12),
  C13(H13), C8(H8)
6.b Fitted hexagon refined as free rotating group:
 C005(N003,C3,C006,C00D,C00C), C00P(C00G,C007,C1,C00N,C00U), C00B(C10,N2,C4,C5,
 C11), C6(C12,C13,C9,C8,C7)
;
_shelx_res_checksum              70414
_shelx_fab_checksum              104
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'