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_1571800
_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_formula_moiety         'C58 H48 Cl N7 Pd2'
_chemical_formula_sum            'C58 H48 Cl N7 Pd2'
_chemical_formula_weight         1091.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-07
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5782(3)
_cell_length_b                   19.0441(4)
_cell_length_c                   16.8698(5)
_cell_measurement_reflns_used    21019
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.9470
_cell_measurement_theta_min      3.4820
_cell_volume                     4683.5(2)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0697
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -32.00  42.00   1.00    3.40    --   34.48 -57.00  30.00   74
  2  \w     22.00  73.00   1.00    3.40    --   34.48 -99.00 120.00   51
  3  \w     24.00  87.00   1.00    3.40    --   34.48-125.00   0.00   63
  4  \w     23.00  86.00   1.00    3.40    --   34.48-125.00 -60.00   63
  5  \w     42.00 132.00   1.00   13.70    --  105.88 -77.00  60.00   90
  6  \w     90.00 116.00   1.00   13.70    --  105.88-111.00  60.00   26
  7  \w     45.00  71.00   1.00   13.70    --  105.88-111.00  60.00   26
  8  \w     37.00 102.00   1.00   13.70    --  105.88 -94.00   0.00   65
  9  \w     53.00 116.00   1.00   13.70    --  105.88-111.00-120.00   63
 10  \w     62.00 132.00   1.00   13.70    --  105.88 -77.00-150.00   70
 11  \w     84.00 136.00   1.00   13.70    --  105.88  30.00   0.00   52
 12  \w    121.00 173.00   1.00   13.70    --  105.88  77.00  30.00   52
 13  \w    137.00 167.00   1.00   13.70    --  105.88  61.00 120.00   30
 14  \w    121.00 170.00   1.00   13.70    --  105.88  77.00  90.00   49
 15  \w    125.00 173.00   1.00   13.70    --  105.88  77.00  60.00   48
 16  \w    129.00 172.00   1.00   13.70    --  105.88  77.00 -30.00   43
 17  \w    125.00 171.00   1.00   13.70    --  105.88  77.00 -60.00   46
 18  \w    123.00 172.00   1.00   13.70    --  105.88  77.00-120.00   49
 19  \w    123.00 173.00   1.00   13.70    --  105.88  77.00-180.00   50
 20  \w    123.00 167.00   1.00   13.70    --  105.88  77.00-150.00   44
 21  \w    117.00 173.00   1.00   13.70    --  105.88  77.00 -90.00   56
 22  \w    120.00 171.00   1.00   13.70    --  105.88  77.00   0.00   51
 23  \w    118.00 164.00   1.00   13.70    --  105.88  77.00 150.00   46
 24  \w     88.00 114.00   1.00   13.70    --  105.88  61.00  90.00   26
 25  \w     88.00 114.00   1.00   13.70    --  105.88  61.00  60.00   26
 26  \w     88.00 114.00   1.00   13.70    --  105.88  61.00  30.00   26
 27  \w     88.00 114.00   1.00   13.70    --  105.88  61.00   0.00   26
 28  \w     85.00 130.00   1.00   13.70    --  105.88  30.00  30.00   45
 29  \w     84.00 113.00   1.00   13.70    --  105.88  30.00 -30.00   29
 30  \w     88.00 114.00   1.00   13.70    --  105.88  61.00 -60.00   26
 31  \w     88.00 115.00   1.00   13.70    --  105.88  61.00 -90.00   27
 32  \w     88.00 114.00   1.00   13.70    --  105.88  61.00-120.00   26
 33  \w     88.00 114.00   1.00   13.70    --  105.88  61.00-150.00   26
 34  \w     89.00 114.00   1.00   13.70    --  105.88  61.00-180.00   25
 35  \w     79.00 105.00   1.00   13.70    --  105.88  77.00-120.00   26
 36  \w     79.00 105.00   1.00   13.70    --  105.88  77.00-150.00   26
 37  \w     79.00 104.00   1.00   13.70    --  105.88  77.00-180.00   25
 38  \w     84.00 113.00   1.00   13.70    --  105.88  30.00-120.00   29
 39  \w     85.00 117.00   1.00   13.70    --  105.88  30.00 -90.00   32
 40  \w     84.00 114.00   1.00   13.70    --  105.88  30.00 -60.00   30
 41  \w     79.00 105.00   1.00   13.70    --  105.88  77.00   0.00   26
 42  \w     79.00 105.00   1.00   13.70    --  105.88  77.00  30.00   26
 43  \w     79.00 105.00   1.00   13.70    --  105.88  77.00  60.00   26
 44  \w     79.00 105.00   1.00   13.70    --  105.88  77.00  90.00   26
 45  \w     88.00 114.00   1.00   13.70    --  105.88  61.00 120.00   26
 46  \w     79.00 105.00   1.00   13.70    --  105.88  77.00 150.00   26
 47  \w     79.00 107.00   1.00   13.70    --  105.88  77.00 120.00   28
 48  \w     84.00 112.00   1.00   13.70    --  105.88  30.00 120.00   28
 49  \w     85.00 113.00   1.00   13.70    --  105.88  30.00 150.00   28
 50  \w     84.00 111.00   1.00   13.70    --  105.88  30.00  90.00   27
 51  \w     84.00 110.00   1.00   13.70    --  105.88  30.00  60.00   26
 52  \w     79.00 105.00   1.00   13.70    --  105.88  77.00 -30.00   26
 53  \w     79.00 105.00   1.00   13.70    --  105.88  77.00 -60.00   26
 54  \w     79.00 105.00   1.00   13.70    --  105.88  77.00 -90.00   26
 55  \w     84.00 110.00   1.00   13.70    --  105.88  30.00-150.00   26
 56  \w     84.00 115.00   1.00   13.70    --  105.88  30.00-180.00   31
 57  \w     74.00 101.00   1.00    3.40    --   34.48  71.00 -27.00   27
 58  \w     18.00  93.00   1.00    3.40    --   34.48  57.00 -30.00   75
 59  \w     14.00  61.00   1.00    3.40    --   34.48  71.00 -27.00   47
 60  \w     16.00 103.00   1.00    3.40    --   34.48  38.00 -90.00   87
 61  \w      8.00  82.00   1.00    3.40    --   34.48  77.00 -90.00   74
 62  \w     -9.00  47.00   1.00    3.40    --   34.48 -57.00 -30.00   56
 63  \w    -32.00  31.00   1.00    3.40    --   34.48 -57.00-180.00   63
 64  \w    -15.00 102.00   1.00    3.40    --   34.48   0.00-180.00  117
 65  \w      9.00  50.00   1.00    3.40    --   34.48  77.00-150.00   41
 66  \w     -2.00  24.00   1.00    3.40    --   34.48  96.00 -55.22   26
 67  \w      9.00  97.00   1.00    3.40    --   34.48  77.00  30.00   88
 68  \w      9.00 100.00   1.00    3.40    --   34.48  77.00 150.00   91
 69  \w      8.00  68.00   1.00    3.40    --   34.48  77.00  90.00   60
 70  \w    -33.00  40.00   1.00    3.40    --   34.48 -38.00  90.00   73
;
_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      0.1055999000
_diffrn_orient_matrix_UB_12      -0.0025509000
_diffrn_orient_matrix_UB_13      0.0025133000
_diffrn_orient_matrix_UB_21      -0.0045389000
_diffrn_orient_matrix_UB_22      -0.0643061000
_diffrn_orient_matrix_UB_23      0.0554080000
_diffrn_orient_matrix_UB_31      0.0003670000
_diffrn_orient_matrix_UB_32      -0.0490625000
_diffrn_orient_matrix_UB_33      -0.0724734000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            59585
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         3.500
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07529
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.512
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0520P)^2^+19.1016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1376
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3877
_reflns_number_total             4276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01909a2.cif
_cod_data_source_block           exp_3204
_cod_depositor_comments
'Adding full bibliography for 1571798--1571800.cif.'
_cod_database_code               1571800
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C100 H100 N6 Pd1 Cl2'
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.537
_reflns_odcompleteness_completeness 100.00
_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. Others
 Fixed Sof: H00E(0.5) H00F(0.5) H00H(0.5) H00I(0.5) H00K(0.5) H01E(0.5)
 H01F(0.5)
3.a Me refined with riding coordinates:
 C00P(H00D,H00E,H00F), C013(H01D,H01E,H01F)
3.b Aromatic/amide H refined with riding coordinates:
 N005(H005), N006(H006), C009(H009), C00G(H00G), C00J(H00J), C00L(H00L),
 C00Q(H00Q), C00T(H00T), C00V(H00V), C00W(H00W), C00Z(H00Z), C011(H011)
3.c Idealised Me refined as rotating group:
 C00E(H00A,H00B,H00C), C00Y(H00H,H00I,H00K), C012(H01A,H01B,H01C), C014(H01G,
 H01H,H01I)
;
_shelx_res_checksum              71061
_shelx_hkl_checksum              5450
_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 7.628
_oxdiff_exptl_absorpt_empirical_full_min 0.542