Synthesis of a macrocyclic oligomer of pyridylbenzoxazole utilizing dynamic covalent bonds and its unsymmetric conversion.
Hokimoto, Yuya; Nakamura, Takashi; Chemical communications (Cambridge, England) 60 (2024) 1281–1284; doi:10.1039/d3cc06216c

data_7132577
_publ_section_title
;
 Synthesis of a macrocyclic oligomer of pyridylbenzoxazole utilizing
 dynamic covalent bonds and its unsymmetric conversion.
;
_journal_issue                   10
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1281
_journal_page_last               1284
_journal_paper_doi               10.1039/d3cc06216c
_journal_volume                  60
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         '(C48 H42 N6 O3), 2(H2 O)'
_chemical_formula_sum            'C48 H46 N6 O5'
_chemical_formula_weight         786.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-11-14 deposited with the CCDC.	2024-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.082(4)
_cell_length_b                   17.555(5)
_cell_length_c                   17.564(5)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.504
_cell_measurement_theta_min      2.319
_cell_volume                     4959(2)
_computing_cell_refinement       'APEX3 (Bruker Nano, 2019)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'APEX3 (Bruker Nano, 2019)'
_computing_publication_material  'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2016/11 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1421
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            92992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        23.255
_diffrn_reflns_theta_max         23.255
_diffrn_reflns_theta_min         1.640
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;    
 SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.820
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Flack x determined using 1719 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.3(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.440
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.440
_refine_ls_R_factor_all          0.1963
_refine_ls_R_factor_gt           0.1644
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3650
_refine_ls_wR_factor_ref         0.3766
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5533
_reflns_number_total             7118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06216c2.cif
_cod_data_source_block           n588c
_cod_depositor_comments
'Adding full bibliography for 7132576--7132579.cif.'
_cod_database_code               7132577
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              86818
_shelx_hkl_checksum              26361