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_7719331
_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
'C56 H52 N8 Pd2, 4(B F4), 1.5(C4 H8 O2), 2(C2 H3 N)'
_chemical_formula_sum            'C66 H70 B4 F16 N10 O3 Pd2'
_chemical_formula_weight         1611.36
_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
_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                90
_cell_angle_beta                 100.215(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7185(11)
_cell_length_b                   29.610(3)
_cell_length_c                   11.7110(13)
_cell_measurement_reflns_used    9603
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.031
_cell_measurement_theta_min      2.289
_cell_volume                     3657.9(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_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      150.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0547
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28914
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.049
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6225
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0999 before and 0.0687 after correction.
The Ratio of minimum to maximum transmission is 0.8349.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8356
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0385P)^2^+8.0706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7087
_reflns_number_total             8356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01592h2.cif
_cod_data_source_block           mo_zq_dwt_449_150k_0m_a
_cod_depositor_comments
'Adding full bibliography for 7719330--7719332.cif.'
_cod_original_cell_volume        3657.8(7)
_cod_database_code               7719331
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.771
_olex2_refinement_description
;
1. Restrained distances
 F5-B2 \\sim F5A-B2
 with sigma of 0.02
 F6-B2 \\sim F6A-B2
 with sigma of 0.02
 F7-B2 \\sim F7A-B2
 with sigma of 0.02
 F8-B2 \\sim F8A-B2
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
F7 \\sim F5A \\sim F5 \\sim F7A \\sim F6 \\sim F6A \\sim F8 \\sim F8A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O1) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(O29)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F6) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F8A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F8) = Uanis(F8A)
Uanis(F6) = Uanis(F6A)
Uanis(F7) = Uanis(F7A)
Uanis(F5A) = Uanis(F5)
3. Others
 Sof(F5A)=Sof(F8A)=Sof(F6A)=Sof(F7A)=1-FVAR(1)
 Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=FVAR(1)
 Fixed Sof: O1(0.75) C27(0.75) H27A(0.75) H27B(0.75) H27C(0.75) C28(0.75)
 O29(0.75) C30(0.75) H30A(0.75) H30B(0.75) C31(0.75) H31A(0.75) H31B(0.75)
 H31C(0.75)
4.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C25(H25A,H25B), C30(H30A,H30B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C9(H9), C10(H10), C11(H11), C15(H15), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21)
4.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              49369
_shelx_hkl_checksum              86458
_olex2_submission_special_instructions 'No special instructions were received'