Solvent-free synthesis and chiroptical properties of a C-N axially chiral cruciform dimer of benzo[<i>b</i>]phenoxazine.
Ishikawa, Shuhei; Sakamaki, Daisuke; Gon, Masayuki; Tanaka, Kazuo; Fujiwara, Hideki; Chemical communications (Cambridge, England) 60 (2024) 4946–4949; doi:10.1039/d4cc00977k

data_7132954
_publ_section_title
;
 Solvent-free synthesis and chiroptical properties of a C-N axially chiral
 cruciform dimer of benzo[<i>b</i>]phenoxazine.
;
_journal_issue                   37
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4946
_journal_page_last               4949
_journal_paper_doi               10.1039/d4cc00977k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C40 H36 N2 O2'
_chemical_formula_sum            'C40 H36 N2 O2'
_chemical_formula_weight         576.74
_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     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2024-02-12 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                87.125(5)
_cell_angle_beta                 64.484(6)
_cell_angle_gamma                67.794(6)
_cell_formula_units_Z            2
_cell_length_a                   12.0197(7)
_cell_length_b                   12.0255(7)
_cell_length_c                   13.0084(8)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100
_cell_measurement_theta_max      77.08
_cell_measurement_theta_min      3.93
_cell_volume                     1556.7(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, ????)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18901
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         77.097
_diffrn_reflns_theta_min         3.800
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             612.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6303
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0828P)^2^+0.3023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5517
_reflns_number_total             6303
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d4cc00977k2.cif
_cod_data_source_block           xcalibur
_cod_depositor_comments
'Adding full bibliography for 7132954--7132956.cif.'
_cod_database_code               7132954
_shelx_res_checksum              69875
_shelx_hkl_checksum              93403