Multi-dimensional microenvironment engineering in heteroleptic coordination cages for programmable biomimetic recognition.
Xie, Xiao-Dan; Bai, Qixia; Zhang, Zhe; Wang, Pingshan; Zhang, Qi; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13783–13788; doi:10.1039/d5dt01757b

data_7719328
_publ_section_title
;
 Multi-dimensional microenvironment engineering in heteroleptic
 coordination cages for programmable biomimetic recognition.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13783
_journal_page_last               13788
_journal_paper_doi               10.1039/d5dt01757b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C67 H51 N11 Pd2, 4(B F4), C2 H3 N'
_chemical_formula_sum            'C69 H54 B4 F16 N12 Pd2'
_chemical_formula_weight         1611.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-05
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-27 deposited with the CCDC.	2025-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                95.9220(10)
_cell_angle_beta                 93.4900(10)
_cell_angle_gamma                98.6030(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9137(2)
_cell_length_b                   18.7121(3)
_cell_length_c                   19.4230(3)
_cell_measurement_reflns_used    9639
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      54.919
_cell_measurement_theta_min      3.599
_cell_volume                     4245.57(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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_temperature      170.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            100515
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.031
_diffrn_reflns_theta_min         3.051
_diffrn_source_current           2.86
_diffrn_source_power             0.1995708
_diffrn_source_voltage           69.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.751
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1143 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.7688.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.397
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         16155
_refine_ls_number_restraints     496
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+7.2019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14347
_reflns_number_total             16155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01757b2.cif
_cod_data_source_block           240905xxd
_cod_depositor_comments
'Adding full bibliography for 7719328--7719329.cif.'
_cod_database_code               7719328
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.652
_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. Restrained distances
 B5-F11 = B5-F12 = B5-F13 = B5-F14
 1.42 with sigma of 0.02
 B3-F9 = B3-F10 = B3-F15 = B3-F16
 1.42 with sigma of 0.02
 B5-F11 \\sim B5-F12 \\sim B5-F13 \\sim B5-F14
 with sigma of 0.02
 F11-F12 \\sim F12-F13 \\sim F13-F14 \\sim F14-F11 \\sim F12-F14 \\sim F11-F13
 with sigma of 0.04
 B5-F11 \\sim B6-F3A
 with sigma of 0.02
 B5-F12 \\sim B6-F4A
 with sigma of 0.02
 B5-F13 \\sim B6-F5A
 with sigma of 0.02
 B5-F14 \\sim B6-F6A
 with sigma of 0.02
 F11-F12 \\sim F3A-F4A
 with sigma of 0.04
 F11-F13 \\sim F3A-F5A
 with sigma of 0.04
 F11-F14 \\sim F3A-F6A
 with sigma of 0.04
 F12-F13 \\sim F4A-F5A
 with sigma of 0.04
 F12-F14 \\sim F4A-F6A
 with sigma of 0.04
 F13-F14 \\sim F5A-F6A
 with sigma of 0.04
 B3-F9 \\sim B3-F10 \\sim B3-F15 \\sim B3-F16
 with sigma of 0.02
 F9-F10 \\sim F10-F15 \\sim F15-F16 \\sim F16-F9 \\sim F10-F16 \\sim F9-F15
 with sigma of 0.04
 B3-F9 \\sim B4-F1A
 with sigma of 0.02
 B3-F10 \\sim B4-F2A
 with sigma of 0.02
 B3-F15 \\sim B4-F7A
 with sigma of 0.02
 B3-F16 \\sim B4-F8A
 with sigma of 0.02
 F9-F10 \\sim F1A-F2A
 with sigma of 0.04
 F9-F15 \\sim F1A-F7A
 with sigma of 0.04
 F9-F16 \\sim F1A-F8A
 with sigma of 0.04
 F10-F15 \\sim F2A-F7A
 with sigma of 0.04
 F10-F16 \\sim F2A-F8A
 with sigma of 0.04
 F15-F16 \\sim F7A-F8A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
F11 \\sim F12 \\sim F13 \\sim F14 \\sim B5: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
F3A \\sim F4A \\sim F5A \\sim F6A \\sim B6 \\sim F11 \\sim F12 \\sim F13 \\sim
F14 \\sim B5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
F9 \\sim F10 \\sim F15 \\sim F16 \\sim B3: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
F1A \\sim F2A \\sim F7A \\sim F8A \\sim B4 \\sim F9 \\sim F10 \\sim F15 \\sim
F16 \\sim B3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
4. Rigid body (RIGU) restrains
 F11, F12, F13, F14, B5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F9, F10, F15, F16, B3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(B6)=1-FVAR(1)
 Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(B5)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F7A)=Sof(F8A)=Sof(B4)=1-FVAR(2)
 Sof(F9)=Sof(F10)=Sof(F15)=Sof(F16)=Sof(B3)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C17(H17), C18(H18),
 C19(H19), C24(H24), C25(H25), C27(H27), C31(H31), C32(H32), C33(H33), C38(H38),
  C39(H39), C41(H41), C45(H45), C46(H46), C48(H48), C52(H52), C53(H53),
 C54(H54), C59(H59), C60(H60), C61(H61)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C67(H67A,
 H67B,H67C), C69(H69A,H69B,H69C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              88728
_shelx_hkl_checksum              32297
_shelx_fab_checksum              7299
_olex2_submission_special_instructions 'No special instructions were received'