Steric engineering of Pd<sup>II</sup>-ligand coordination pathways: hierarchical control from functionally addressable intermediates to supramolecular architectures.
Tang, Ao; Dai, Wen-Tao; Bai, Qixia; Xie, Xiao-Dan; Zhang, Zhe; Wang, Pingshan; Lu, Wei; Zhang, Qi; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13759–13763; doi:10.1039/d5dt01592h

data_7719330
_publ_section_title
;
 Steric engineering of Pd<sup>II</sup>-ligand coordination pathways:
 hierarchical control from functionally addressable intermediates to
 supramolecular architectures.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13759
_journal_page_last               13763
_journal_paper_doi               10.1039/d5dt01592h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C60 H60 N8 Pd2, 4(B F4), 8(C2 H3 N)'
_chemical_formula_sum            'C76 H84 B4 F16 N16 Pd2'
_chemical_formula_weight         1781.63
_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
_audit_creation_date             2025-07-23
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-23 deposited with the CCDC.	2025-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                77.772(2)
_cell_angle_beta                 75.568(2)
_cell_angle_gamma                68.003(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9441(6)
_cell_length_b                   13.9935(8)
_cell_length_c                   15.8444(9)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.29
_cell_measurement_theta_min      2.91
_cell_volume                     2159.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23971
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.281
_diffrn_reflns_theta_min         2.905
_exptl_absorpt_coefficient_mu    4.083
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.2192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1587 before and 0.0880 after correction.
The Ratio of minimum to maximum transmission is 0.2911.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.592
_refine_diff_density_min         -2.346
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         7773
_refine_ls_number_restraints     543
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0635
_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^)+(0.1367P)^2^+0.3855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.1809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7228
_reflns_number_total             7773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01592h2.cif
_cod_data_source_block           cu_zq_dwt_470_150k_0m_a
_cod_depositor_comments
'Adding full bibliography for 7719330--7719332.cif.'
_cod_database_code               7719330
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.454
_shelx_estimated_absorpt_t_min   0.235
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
: with sigma of 0.01 and sigma for terminal atoms of 0.02
2. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Same fragment restrains
4. Others
 Sof(B1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=1-FVAR(1)
 Sof(B1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=FVAR(1)
 Sof(N1)=Sof(C2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(2)
 Sof(N1)=Sof(C2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C26(H26)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12), C16(H16),
 C17(H17), C19(H19)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C3(H3A,H3B,H3C), C3(H3A,H3B,
 H3C), C3(H3A,H3B,H3C), C3(H3A,H3B,H3C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              34178
_shelx_hkl_checksum              67654
_olex2_submission_special_instructions 'No special instructions were received'