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_7132840
_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, 0.5(C6 H5 Cl), F6 P'
_chemical_formula_sum            'C47 H20.5 Cl0.5 F16 N3 P Pd S'
_chemical_formula_weight         1118.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-07-12 deposited with the CCDC.	2024-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.140(11)
_cell_length_b                   14.513(9)
_cell_length_c                   20.554(10)
_cell_measurement_reflns_used    240860
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      15.579
_cell_measurement_theta_min      0.842
_cell_volume                     8394(7)
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Pilatus3 CdTe 1M'
_diffrn_measurement_method       \w
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.41360
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            240860
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        14.369
_diffrn_reflns_theta_max         15.579
_diffrn_reflns_theta_min         0.842
_diffrn_source                   'BL02B1 beamline SPring-8'
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
PROCESS-AUTO (1998). Automatic Data Acquisition and Processing Package
for 2D image data. Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4424
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 8068 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.413(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1252
_refine_ls_number_reflns         19243
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0535P)^2^+8.3185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                18113
_reflns_number_total             19243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00806e2.cif
_cod_data_source_block           mf-37-1_a
_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_formula_sum        'C47 H20.50 Cl0.50 F16 N3 P Pd S'
_cod_database_code               7132840
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.943
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              65734
_shelx_hkl_checksum              90642