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_1571798
_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         'Cl, C H Cl3, C58 H52 N7, 2(C2 H3 N)'
_chemical_formula_sum            'C63 H59 Cl4 N9'
_chemical_formula_weight         1083.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-14
_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                 91.717(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7069(7)
_cell_length_b                   16.7483(6)
_cell_length_c                   31.0611(12)
_cell_measurement_reflns_used    5737
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      71.7110
_cell_measurement_theta_min      2.9810
_cell_volume                     5567.4(5)
_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      99.9(5)
_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     -7.00  40.00   1.00    2.00    --   34.73 -77.00  30.00   47
  2  \w     26.00  88.00   1.00    2.00    --   34.73-125.00 -30.00   62
  3  \w     44.00 121.00   1.00    6.00    --  105.88 -45.00 -90.00   77
  4  \w     58.00  84.00   1.00    6.00    --  105.88 -94.00   0.00   26
  5  \w     44.00 139.00   1.00    6.00    --  105.88 -15.00 -60.00   95
  6  \w     97.00 165.00   1.00    6.00    --  105.88  51.00 -57.00   68
  7  \w    106.00 172.00   1.00    6.00    --  105.88  61.00 -30.00   66
  8  \w    108.00 175.00   1.00    6.00    --  105.88 111.00-180.00   67
  9  \w     13.00  40.00   1.00    2.00    --   34.73 -99.00 -60.00   27
 10  \w      5.00  56.00   1.00    2.00    --   34.73 -99.00-120.00   51
 11  \w    -27.00  51.00   1.00    2.00    --   34.73 -57.00 120.00   78
 12  \w     41.00 127.00   1.00    6.00    --  105.88 -30.00 150.00   86
 13  \w    -97.00 -25.00   1.00    2.00    --  -34.73 -38.00 -90.00   72
;
_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      0.0100508000
_diffrn_orient_matrix_UB_12      -0.0367573000
_diffrn_orient_matrix_UB_13      -0.0453128000
_diffrn_orient_matrix_UB_21      0.1191527000
_diffrn_orient_matrix_UB_22      -0.0449787000
_diffrn_orient_matrix_UB_23      0.0149106000
_diffrn_orient_matrix_UB_31      -0.0803818000
_diffrn_orient_matrix_UB_32      -0.0712171000
_diffrn_orient_matrix_UB_33      0.0136607000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            20151
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.593
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         2.847
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.315
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41247
_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    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.729
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         9836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0729
_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^)+(0.0816P)^2^+10.3701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1843
_refine_ls_wR_factor_ref         0.1975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7729
_reflns_number_total             9836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01909a2.cif
_cod_data_source_block           exp_2723
_cod_depositor_comments
'Adding full bibliography for 1571798--1571800.cif.'
_cod_database_code               1571798
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C100 H100 N7'
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.655
_reflns_odcompleteness_completeness 99.97
_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 Ternary CH refined with riding coordinates:
 C60(H60)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7A), C8(H8), C48(H48), C21(H21), C13(H13), C17(H17), C3(H3),
 C25(H25), C12(H12), C20(H20), C46(H46), C40(H40), C16(H16), C42(H42), C34(H34),
  C30(H30), C29(H29), C26(H26), C36(H36), C2(H2A)
2.c Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C51(H51A,H51B,
 H51C), C54(H54A,H54B,H54C), C58(H58A,H58B,H58C), C56(H56A,H56B,H56C), C53(H53A,
 H53B,H53C), C52(H52A,H52B,H52C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              40212
_shelx_hkl_checksum              50945
_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 1.953
_oxdiff_exptl_absorpt_empirical_full_min 0.708