Cyclo[4]pyrrole with <i>α</i>-<i>β</i> direct linkages.
Sun, Yuhua; Kitahara, Riku; Ichino, Tomoya; Ide, Yuki; Senboku, Hisanori; Shimizu, Soji; Tanaka, Takayuki; Inokuma, Yasuhide; Chemical science 15 (2024) 19571–19576; doi:10.1039/d4sc06670g

data_1573043
_publ_section_title
;
 Cyclo[4]pyrrole with <i>&#x3b1;</i>-<i>&#x3b2;</i> direct linkages.
;
_journal_issue                   46
_journal_name_full               'Chemical science'
_journal_page_first              19571
_journal_page_last               19576
_journal_paper_doi               10.1039/d4sc06670g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C28 H36 N4'
_chemical_formula_sum            'C28 H36 N4'
_chemical_formula_weight         428.61
_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   mixed
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2024-09-10 deposited with the CCDC.	2024-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                62.149(6)
_cell_angle_beta                 61.589(7)
_cell_angle_gamma                65.472(7)
_cell_formula_units_Z            1
_cell_length_a                   9.0906(8)
_cell_length_b                   9.1054(5)
_cell_length_c                   9.2735(5)
_cell_measurement_reflns_used    3346
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.8510
_cell_measurement_theta_min      2.5900
_cell_volume                     578.30(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6420
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.612
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0464P)^2^+0.2646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2268
_reflns_number_total             2429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06670g2.cif
_cod_data_source_block           cmpd_3
_cod_depositor_comments
'Adding full bibliography for 1573043--1573044.cif.'
_cod_original_cell_volume        578.30(9)
_cod_database_code               1573043
_shelx_shelxl_version_number     2019/2
_oxdiff_exptl_absorpt_empirical_full_min 0.822
_oxdiff_exptl_absorpt_empirical_full_max 1.738
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              86046
_shelx_hkl_checksum              55715