Mono- and bis-Pd(ii) complexes of N-confused dithiahexaphyrin(1.1.1.1.1.0) with the absorption and aromaticity modulated by Pd(ii) coordination, macrocycle contraction and ancillary ligands.
Sun, Meng; Xie, Yongshu; Baryshnikov, Glib; Li, Chengjie; Sha, Feng; Wu, Xinyan; Ågren, Hans; Li, Shijun; Li, Qizhao; Chemical science 15 (2024) 2047–2054; doi:10.1039/d3sc05473j

data_1570647
_publ_section_title
;
 Mono- and bis-Pd(ii) complexes of N-confused
 dithiahexaphyrin(1.1.1.1.1.0) with the absorption and aromaticity
 modulated by Pd(ii) coordination, macrocycle contraction and ancillary
 ligands.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              2047
_journal_page_last               2054
_journal_paper_doi               10.1039/d3sc05473j
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C77 H27 Cl F25 N4 O P Pd S2'
_chemical_formula_sum            'C77 H27 Cl F25 N4 O P Pd S2'
_chemical_formula_weight         1735.96
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-07
_audit_creation_method
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_audit_update_record
;
2023-06-27 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                70.416(3)
_cell_angle_beta                 65.162(2)
_cell_angle_gamma                76.985(3)
_cell_formula_units_Z            2
_cell_length_a                   16.9156(14)
_cell_length_b                   17.3251(16)
_cell_length_c                   19.0029(17)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    213
_cell_measurement_theta_max      54.967
_cell_measurement_theta_min      4.624
_cell_volume                     4738.3(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      213
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_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  0.0736
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            102513
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.518
_diffrn_reflns_theta_min         2.497
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5471
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1013
_refine_ls_number_reflns         21690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17568
_reflns_number_total             21690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05473j2.cif
_cod_data_source_block           mo_d8v22326_0m
_cod_depositor_comments
'Adding full bibliography for 1570646--1570650.cif.'
_cod_database_code               1570647
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.943
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups 
2.a Aromatic/amide H refined with riding coordinates: 
 C2(H2), C3(H3A), C7(H7), C12(H12), C13(H13), C17(H17), C18(H18), C22(H22), 
 C23(H23), C26(H26), C27(H27), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), 
  C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C74(H74), C75(H75), 
 C76(H76), C77(H77), C78(H78) 
;
_shelx_res_checksum              98950
_shelx_hkl_checksum              71793
_shelx_fab_checksum              25917
_olex2_submission_special_instructions 'No special instructions were received'