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_1570648
_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         'C59 H11 F25 N4 O Pd S2'
_chemical_formula_sum            'C59 H11 F25 N4 O Pd S2'
_chemical_formula_weight         1437.24
_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             2022-04-22
_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                113.418(4)
_cell_angle_beta                 96.893(4)
_cell_angle_gamma                108.505(4)
_cell_formula_units_Z            2
_cell_length_a                   12.633(2)
_cell_length_b                   16.870(3)
_cell_length_c                   18.510(3)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      53.448
_cell_measurement_theta_min      4.532
_cell_volume                     3292.5(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.946
_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  0.0825
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41905
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.857
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;

;
_refine_diff_density_max         1.016
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         10934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0708
_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^)+(0.1245P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.2058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6826
_reflns_number_total             10934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05473j2.cif
_cod_data_source_block           mo_ddz21054_0m
_cod_depositor_comments
'Adding full bibliography for 1570646--1570650.cif.'
_cod_original_cell_volume        3292.4(10)
_cod_database_code               1570648
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.947
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C2(H2), C3(H3A), C6(H6), C11(H11), C12(H12), C16(H16), C17(H17),
 C22(H22), C26(H26), C27(H27)
;
_shelx_res_checksum              2722
_shelx_hkl_checksum              85306
_olex2_submission_special_instructions 'No special instructions were received'