The unprecedented strong paratropic ring current of a bis-Pd<sup>II</sup> complex of 5,10,23-trimesityl [28]heptaphyrin(1.1.0.0.1.0.0).
Liu, Yang; Xu, Ling; Jin, Xiaorong; Yin, Bangshao; Rao, Yutao; Zhou, Mingbo; Song, Jianxin; Osuka, Atsuhiro; Chemical science 15 (2024) 11402–11407; doi:10.1039/d4sc01909a

data_1571799
_publ_section_title
;
 The unprecedented strong paratropic ring current of a bis-Pd<sup>II</sup>
 complex of 5,10,23-trimesityl [28]heptaphyrin(1.1.0.0.1.0.0).
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              11402
_journal_page_last               11407
_journal_paper_doi               10.1039/d4sc01909a
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C58 H50 B F2 N7'
_chemical_formula_sum            'C58 H50 B F2 N7'
_chemical_formula_weight         893.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-02-01 deposited with the CCDC.	2024-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.272(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9268(3)
_cell_length_b                   27.7816(9)
_cell_length_c                   16.3663(5)
_cell_measurement_reflns_used    3951
_cell_measurement_temperature    100.0(9)
_cell_measurement_theta_max      70.8390
_cell_measurement_theta_min      2.7930
_cell_volume                     5231.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 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_environment      N~2~
_diffrn_ambient_temperature      100.0(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0697
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -37.00  32.00   1.00    5.00    --  -34.73  57.00   0.00   69
  2  \w     63.00 102.00   1.00    5.00    --   34.73  38.00 120.00   39
  3  \w    -31.00  39.00   1.00    5.00    --   34.73 -57.00-150.00   70
  4  \w     13.00  66.00   1.00    5.00    --   34.73 -99.00  90.00   53
  5  \w     36.00  63.00   1.00    5.00    --   34.73-125.00   0.00   27
  6  \w     24.00  57.00   1.00    5.00    --   34.73-125.00-150.00   33
  7  \w     76.00 104.00   1.00    5.00    --   34.73  38.00 -90.00   28
  8  \w     69.00 103.00   1.00   20.00    --  105.25 -94.00-180.00   34
  9  \w     36.00  88.00   1.00   20.00    --  105.25 -94.00 150.00   52
 10  \w    148.00 176.00   1.00   20.00    --  105.25  15.00-150.00   28
 11  \w     42.00 119.00   1.00   20.00    --  105.25 -45.00 150.00   77
 12  \w     88.00 174.00   1.00   20.00    --  105.25  45.00 -90.00   86
 13  \w    115.00 165.00   1.00   20.00    --  105.25  61.00   0.00   50
 14  \w     46.00 119.00   1.00   20.00    --  105.25 -45.00 -90.00   73
 15  \w     60.00 107.00   1.00   20.00    --  105.25 -45.00   0.00   47
 16  \w     74.00 124.00   1.00   20.00    --  105.25  15.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0560109000
_diffrn_orient_matrix_UB_12      -0.0421405000
_diffrn_orient_matrix_UB_13      0.0362441000
_diffrn_orient_matrix_UB_21      -0.0489451000
_diffrn_orient_matrix_UB_22      -0.0200988000
_diffrn_orient_matrix_UB_23      -0.0901023000
_diffrn_orient_matrix_UB_31      0.1113259000
_diffrn_orient_matrix_UB_32      -0.0298994000
_diffrn_orient_matrix_UB_33      0.0094220000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.1002
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19567
_diffrn_reflns_point_group_measured_fraction_full 0.729
_diffrn_reflns_point_group_measured_fraction_max 0.729
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         2.799
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       plate
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 2240 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.9(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1243
_refine_ls_number_reflns         13478
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0770P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1724
_reflns_Friedel_coverage         0.426
_reflns_Friedel_fraction_full    0.446
_reflns_Friedel_fraction_max     0.446
_reflns_number_gt                10045
_reflns_number_total             13478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01909a2.cif
_cod_data_source_block           exp_2740_sq
_cod_depositor_comments
;
Adding full bibliography for 1571798--1571800.cif.

2025-06-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C116 H100 B2 F4 N14'
_cod_original_formula_weight         1787.71
_cod_original_formula_moiety         '2(C58 H50 B F2 N7)'
_cod_original_formula_units_Z            2
_cod_database_code               1571799
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C50 H100 N7 B1 F2'
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.945
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), C3(H3), C4(H4A), C7(H7), C8(H8), C11(H11), C12(H12),
 C16(H16), C17(H17), C21(H21), C22(H22), C25(H25), C26(H26), C29(H29), C30(H30),
  C34(H34), C36(H36), C42(H42), C44(H44), C51(H51), C53(H53), N1AA(H1AA),
 N3AA(H3AA), N5AA(H5AA), C61(H61), C62(H62), C65(H65), C66(H66), C69(H69),
 C70(H70), C74(H74), C75(H75), C79(H79), C80(H80), C83(H83), C84(H84), C87(H87),
  C88(H88), C92(H92), C94(H94), C101(H101), C103(H103), C109(H109), C112(H112)
2.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C), C57(H57A,H57B,H57C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C),
 C97(H97A,H97B,H97C), C104(H10A,H10B,H10C), C105(H10D,H10E,H10F), C106(H10G,
 H10H,H10I), C111(H11A,H11B,H11C), C114(H11D,H11E,H11F), C115(H11G,H11H,H11I)
;
_shelx_res_checksum              96597
_shelx_hkl_checksum              44907
_shelx_fab_checksum              73459
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.484
_oxdiff_exptl_absorpt_empirical_full_min 0.822