Short-step synthesis and chiroptical properties of polyaza[5]-[9]helicenes with blue to green-colour emission.
Otani, Takashi; Sasayama, Takuma; Iwashimizu, Chisaki; Kanyiva, Kyalo Stephen; Kawai, Hidetoshi; Shibata, Takanori; Chemical communications (Cambridge, England) 56 (2020) 4484–4487; doi:10.1039/d0cc01194k

data_7126179
_publ_section_title
;
 Short-step synthesis and chiroptical properties of
 polyaza[5]-[9]helicenes with blue to green-colour emission.
;
_journal_issue                   32
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4484
_journal_page_last               4487
_journal_paper_doi               10.1039/d0cc01194k
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C16 H10 N4'
_chemical_formula_sum            'C16 H10 N4'
_chemical_formula_weight         258.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2020-01-23 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.273(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   11.6524(7)
_cell_length_b                   4.0000(2)
_cell_length_c                   14.3571(8)
_cell_measurement_reflns_used    6834
_cell_measurement_temperature    296
_cell_measurement_theta_max      68.05
_cell_measurement_theta_min      3.08
_cell_volume                     668.65(6)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2.4'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6812
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.045
_diffrn_reflns_theta_min         4.796
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             536.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.11
_refine_diff_density_min         -0.60
_refine_ls_abs_structure_details
;
 Flack x determined using 941 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2366
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1641
_refine_ls_R_factor_gt           0.1609
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4010
_refine_ls_wR_factor_ref         0.4065
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                2181
_reflns_number_total             2366
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d0cc01194k2.cif
_cod_data_source_block           20181115-5helicene-2
_cod_depositor_comments
;
Adding full bibliography for 7126178--7126180.cif.

2025-01-30
Z value fixed to be consistent with given formula
                 miguel
;
_cod_original_formula_units_Z            4
_cod_original_cell_volume        668.66(7)
_cod_database_code               7126179
_shelxl_version_number           2014/6
_shelx_res_checksum              54286