Diamond lattice in single-component molecular crystals comprising tetrabenzoporphyrin neutral radicals.
Mine, Kosuke; Arae, Sachie; Murakawa, Hiroshi; Tsuchiizu, Masahisa; Hanasaki, Noriaki; Matsuda, Masaki; Chemical communications (Cambridge, England) 60 (2024) 3019–3022; doi:10.1039/d3cc05948k

data_7132665
_publ_section_title
;
 Diamond lattice in single-component molecular crystals comprising
 tetrabenzoporphyrin neutral radicals.
;
_journal_issue                   22
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3019
_journal_page_last               3022
_journal_paper_doi               10.1039/d3cc05948k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C38 H20 Fe N6'
_chemical_formula_sum            'C38 H20 Fe N6'
_chemical_formula_weight         616.45
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-11-30 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7275(3)
_cell_length_b                   13.7275(3)
_cell_length_c                   14.5027(7)
_cell_measurement_reflns_used    4095
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7790
_cell_measurement_theta_min      2.0380
_cell_volume                     2732.95(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.953
_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      0.00  25.00   0.50  144.23    --   12.27-112.00 -87.00   50
  2  \w    -77.00  -7.00   0.50  144.23    --  -12.43 -14.00  52.00  140
  3  \w     13.00  45.00   0.50  144.23    --   12.27-125.00-120.00   64
  4  \w    -12.00  20.00   0.50  144.23    --   12.27  77.00   0.00   64
  5  \w    -41.00  17.00   0.50  144.23    --   12.27 -77.00  60.00  116
  6  \w    -41.00  13.00   0.50  144.23    --  -12.43 -77.00 -30.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0343020000
_diffrn_orient_matrix_UB_12      0.0070602000
_diffrn_orient_matrix_UB_13      -0.0359099000
_diffrn_orient_matrix_UB_21      -0.0386599000
_diffrn_orient_matrix_UB_22      -0.0065990000
_diffrn_orient_matrix_UB_23      0.0318766000
_diffrn_orient_matrix_UB_31      -0.0002538000
_diffrn_orient_matrix_UB_32      0.0507789000
_diffrn_orient_matrix_UB_33      0.0091202000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6559
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.065
_diffrn_reflns_theta_min         2.043
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0555P)^2^+1.6355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1161
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1220
_reflns_number_total             1586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05948k2.cif
_cod_data_source_block           FetbpCN2
_cod_depositor_comments
'Adding full bibliography for 7132664--7132666.cif.'
_cod_original_cell_volume        2732.95(18)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7132665
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C38H20N6Fe
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9)
;
_shelx_res_checksum              43171
_shelx_hkl_checksum              71498
_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 1.440
_oxdiff_exptl_absorpt_empirical_full_min 0.750