Substitution-pattern- and counteranion-dependent ion-pairing assemblies of heteroporphyrin-based π-electronic cations.
Fujita, Masaki; Haketa, Yohei; Seki, Shu; Maeda, Hiromitsu; Chemical communications (Cambridge, England) 60 (2024) 4190–4193; doi:10.1039/d4cc00806e

data_7132835
_publ_section_title
;
 Substitution-pattern- and counteranion-dependent ion-pairing assemblies
 of heteroporphyrin-based &#x3c0;-electronic cations.
;
_journal_issue                   31
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4190
_journal_page_last               4193
_journal_paper_doi               10.1039/d4cc00806e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'C44 H18 F10 N3 Pd S, C10 N5, C0.83 H1.65 Cl1.65, 0.828(C H2 Cl2)'
_chemical_formula_sum            'C55.66 H21.3 Cl3.31 F10 N8 Pd S'
_chemical_formula_weight         1247.59
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-02-16 deposited with the CCDC.	2024-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.166(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3831(3)
_cell_length_b                   7.1785(2)
_cell_length_c                   26.0801(5)
_cell_measurement_reflns_used    29396
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.161
_cell_measurement_theta_min      1.741
_cell_volume                     2501.71(10)
_computing_cell_refinement
'CrysAlis PRO (Rigaku Oxford Diffraction, 2023)'
_computing_data_collection
'CrysAlis PRO (Rigaku Oxford Diffraction, 2023)'
_computing_data_reduction
'CrysAlis PRO (Rigaku Oxford Diffraction, 2023)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'DECTRIS EIGER X 1M'
_diffrn_measurement_method       'Shutterless \w scans'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.8120
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            29396
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        29.157
_diffrn_reflns_theta_max         33.161
_diffrn_reflns_theta_min         1.741
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75837
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1239
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.288
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 3236 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         10962
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0881P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.785
_reflns_number_gt                8908
_reflns_number_total             10962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00806e2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7132834--7132840.cif.
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C55.66 H21.30 Cl3.31 F10 N8 Pd S'
_cod_database_code               7132835
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_shelx_res_checksum              84308
_shelx_hkl_checksum              48432