Trioxazolo[2^3^]metacyclophane: synthesis, structural analysis, and optical properties
Yu, Hao; Gray, Danielle L.; Woods, Toby J.; Moore, Jeffrey S.; Acta Crystallographica Section C 78 (2022) –; doi:10.1107/S2053229622000298

data_2022515
_publ_section_title
;
 Trioxazolo[2^3^]metacyclophane: synthesis, structural analysis, and
 optical properties
;
_journal_coeditor_code           EQ3005
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229622000298
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'C27 H15 N3 O3'
_chemical_formula_moiety         'C27 H15 N3 O3'
_chemical_formula_sum            'C27 H15 N3 O3'
_chemical_formula_weight         429.42
_chemical_name_common
;
Trioxazolo[2^3^]metacyclophane
;
_chemical_name_systematic
;
Trioxazolo[2^3^]metacyclophane
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.3606(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1863(4)
_cell_length_b                   7.4446(2)
_cell_length_c                   18.3380(5)
_cell_measurement_reflns_used    14248
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.64
_cell_volume                     1936.66(9)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT  (Bruker, 2014), XPREP (Bruker, 2014) and SADABS (Krause
<i>et al.</i>, 2015)
;
_computing_molecular_graphics
;
SHELXTL (Bruker, 2014) and CrystalMaker (Palmer, 2014)
;
_computing_publication_material
;
XCIF (Bruker, 2014)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29490
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.374
_diffrn_reflns_theta_min         2.637
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.99447
_exptl_absorpt_correction_T_min  0.97629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.348
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.215
_refine_ls_extinction_coef       0.0238(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0321P)^2^+1.4734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                3059
_reflns_number_total             3543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eq3005sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2022515
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.991
_shelx_hkl_checksum              95765
_shelx_res_checksum              38857
_cod_database_fobs_code 2022515