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_1573044
_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 H37 N3 O2'
_chemical_formula_sum            'C28 H37 N3 O2'
_chemical_formula_weight         447.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 91.632(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8130(5)
_cell_length_b                   13.3344(5)
_cell_length_c                   14.2787(6)
_cell_measurement_reflns_used    8863
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.4530
_cell_measurement_theta_min      2.0970
_cell_volume                     2438.58(17)
_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 1.000
_diffrn_measured_fraction_theta_max 0.785
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.785
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20678
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.785
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.730
_diffrn_reflns_theta_min         2.090
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56654
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0582P)^2^+0.8654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5076
_reflns_number_total             5970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06670g2.cif
_cod_data_source_block           cmpd_10
_cod_depositor_comments
'Adding full bibliography for 1573043--1573044.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1573044
_shelx_shelxl_version_number     2019/2
_oxdiff_exptl_absorpt_empirical_full_min 0.652
_oxdiff_exptl_absorpt_empirical_full_max 1.437
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              52761
_shelx_hkl_checksum              2077