Synthesis of fully fused tetrapyrazinoporphyrazine polymers bearing three-dimensional structures controlled by steric repulsion.
Watanabe, Kosuke; Toya, Teruki; Toyota, Yuto; Kobayashi, Yoichi; Usuba, Junichi; Hijikata, Yuh; Matsuda, Ryotaro; Nishimura, Katsuyuki; Sugiyama, Haruki; Segawa, Yasutomo; Chemical communications (Cambridge, England) 61 (2025) 2822–2825; doi:10.1039/d4cc06293k

data_7134182
_publ_section_title
;
 Synthesis of fully fused tetrapyrazinoporphyrazine polymers bearing
 three-dimensional structures controlled by steric repulsion.
;
_journal_issue                   13
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2822
_journal_page_last               2825
_journal_paper_doi               10.1039/d4cc06293k
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C40 H42 N10'
_chemical_formula_sum            'C40 H42 N10'
_chemical_formula_weight         662.83
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-05-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-11-15 deposited with the CCDC.	2025-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.561(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.1684(8)
_cell_length_b                   9.2231(4)
_cell_length_c                   12.1013(6)
_cell_measurement_reflns_used    4816
_cell_measurement_temperature    143
_cell_measurement_theta_max      31.2280
_cell_measurement_theta_min      2.8440
_cell_volume                     1816.52(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      143.0
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.850
_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    -15.00  84.00   0.50  190.00    --   12.51  77.00 -60.00  198
  2  \w     16.00  42.00   0.50  190.00    --   12.51  57.00 -90.00   52
  3  \w     39.00  81.00   0.50  190.00    --   12.51 179.00-150.00   84
  4  \w     40.00  91.00   0.50  190.00    --   12.51 179.00  30.00  102
  5  \w     39.00  72.00   0.50  190.00    --   12.51 179.00  60.00   66
  6  \w    -56.00 -31.00   0.50  190.00    --  -11.11 109.00-149.00   50
  7  \w      7.00  57.00   0.50  190.00    --   12.51-109.00 114.00  100
  8  \w      3.00  52.00   0.50  190.00    --   12.51 -99.00-150.00   98
  9  \w    -74.00 -49.00   0.50  190.00    --  -11.11 179.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20618
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         31.286
_diffrn_reflns_theta_min         2.503
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         5050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0726P)^2^+0.1648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2952
_reflns_number_total             5050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06293k3.cif
_cod_data_source_block           3c
_cod_depositor_comments
'Adding full bibliography for 7134179--7134182.cif.'
_cod_database_code               7134182
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C14(H14), C20(H20)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C19(H19A,H19B,
 H19C), C12(H12A,H12B,H12C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              43098
_shelx_hkl_checksum              68735
_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
;