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_7134179
_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         '2(C4 H9 N O), C30 H22 N10'
_chemical_formula_sum            'C38 H40 N12 O2'
_chemical_formula_weight         696.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                107.517(5)
_cell_angle_beta                 91.562(4)
_cell_angle_gamma                116.601(6)
_cell_formula_units_Z            1
_cell_length_a                   9.9056(6)
_cell_length_b                   10.0760(6)
_cell_length_c                   10.9491(5)
_cell_measurement_reflns_used    4941
_cell_measurement_temperature    143
_cell_measurement_theta_max      31.2420
_cell_measurement_theta_min      2.4990
_cell_volume                     914.85(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.829
_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    -53.00  31.00   0.50    1.01    --   12.67 -31.00 -74.00  168
  2  \w    -52.00  -8.00   0.50    1.01    --  -11.26 -57.00-180.00   88
  3  \w     53.00  85.00   0.50    1.01    --   12.67 179.00-180.00   64
  4  \w    -84.00 -44.00   0.50    1.01    --  -11.26 179.00 120.00   80
  5  \w    -11.00  73.00   0.50    1.01    --   12.67  31.00  84.00  168
  6  \w    -15.00  80.00   0.50    1.01    --   12.67  77.00 120.00  190
  7  \w     16.00  50.00   0.50    1.01    --   12.67 -99.00   0.00   68
  8  \w     -9.00  52.00   0.50    1.01    --   12.67 -99.00 -60.00  122
  9  \w    -74.00 -48.00   0.50    1.01    --  -11.26-179.00-120.00   52
;
_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  0.0461
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.829
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13568
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         31.335
_diffrn_reflns_theta_min         2.532
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0563P)^2^+0.0751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3284
_reflns_number_total             4973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06293k3.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 7134179--7134182.cif.'
_cod_original_cell_volume        914.85(10)
_cod_database_code               7134179
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.992
_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. Others
 Sof(O21)=Sof(C22)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(N24)=Sof(C26)=
 Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=1-FVAR(1)
 Sof(O27)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(N30)=Sof(C32)=Sof(H32A)=
 Sof(H32B)=Sof(H32C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C28)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C18(H18)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C17(H17A,H17B,
 H17C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C23(H23A,H23B,H23C), C26(H26A,
 H26B,H26C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              98527
_shelx_hkl_checksum              53890
_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
;