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_7134180
_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         'C22 H22 N10'
_chemical_formula_sum            'C22 H22 N10'
_chemical_formula_weight         426.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6557(5)
_cell_length_b                   14.4716(8)
_cell_length_c                   17.0096(9)
_cell_measurement_reflns_used    4452
_cell_measurement_temperature    143
_cell_measurement_theta_max      30.7410
_cell_measurement_theta_min      2.8390
_cell_volume                     2130.7(2)
_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 0.847
_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    -41.00  37.00   0.50    2.94    --   12.67 -29.00-127.00  156
  2  \w     -3.00  52.00   0.50    2.94    --   12.67 -99.00-180.00  110
  3  \w     18.00  44.00   0.50    2.94    --   12.67 -99.00   0.00   52
  4  \w      9.00  46.00   0.50    2.94    --  -11.26  57.00-120.00   74
;
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11471
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         31.425
_diffrn_reflns_theta_min         2.815
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72025
_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    1.330
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0560P)^2^+0.5806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2026
_reflns_number_total             2981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06293k3.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 7134179--7134182.cif.'
_cod_database_code               7134180
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Others
 Sof(H12A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C13)=Sof(H13A)=Sof(H13B)=1-FVAR(1)
 Sof(H12)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C18)=
 Sof(H18A)=Sof(H18B)=Sof(C17)=Sof(H17A)=Sof(H17B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C12(H12), C12(H12A)
3.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C17(H17A,H17B), C15(H15A,H15B), C13(H13A,H13B)
3.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C16(H16D,H16E,H16F), C14(H14A,H14B,H14C), C14(H14D,H14E,
 H14F)
;
_shelx_res_checksum              21185
_shelx_hkl_checksum              71445
_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
;