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_1570650
_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         'C83 H30 F25 N4 O P Pd2 S2, 2(C2 H3 N)'
_chemical_formula_sum            'C87 H36 F25 N6 O P Pd2 S2'
_chemical_formula_weight         1964.192
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2023-05-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-06-27 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                106.814(4)
_cell_angle_beta                 90.699(5)
_cell_angle_gamma                107.905(4)
_cell_formula_units_Z            2
_cell_length_a                   14.977(2)
_cell_length_b                   16.782(2)
_cell_length_c                   16.991(2)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.46
_cell_volume                     3866.0(8)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      213.15
_diffrn_measured_fraction_theta_full 0.9919
_diffrn_measured_fraction_theta_max 0.9803
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_Laue_measured_fraction_full 0.9919
_diffrn_reflns_Laue_measured_fraction_max 0.9803
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17322
_diffrn_reflns_point_group_measured_fraction_full 0.9919
_diffrn_reflns_point_group_measured_fraction_max 0.9803
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.89
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2950
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1611 before and 0.0895 after correction.
The Ratio of minimum to maximum transmission is 0.3957.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1942.157
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.4807
_refine_diff_density_min         -1.7310
_refine_diff_density_rms         0.1877
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             10.7914
_refine_ls_goodness_of_fit_ref   1.0337
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     1119
_refine_ls_number_reflns         14897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0337
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.0052
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+10.4926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.1715
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              19
_reflns_limit_k_min              -20
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                11458
_reflns_number_total             14897
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc05473j2.cif
_cod_data_source_block           mo_d8v22259_0m
_cod_depositor_comments
'Adding full bibliography for 1570646--1570650.cif.'
_cod_original_cell_volume        3866.0(9)
_cod_database_code               1570650
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C13(H13), C17(H17), C18(H18), C22(H22),
 C23(H23), C26(H26), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C67(H67),
  C68(H68), C69(H69), C70(H70), C71(H71), C73(H73), C74(H74), C75(H75),
 C76(H76), C77(H77), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83)
2.b Idealised Me refined as rotating group:
 C85(H85a,H85b,H85c), C87(H87a,H87b,H87c)
;
_olex2_submission_special_instructions 'No special instructions were received'