B,N-doped PAHs from Tridentate ‘Defects’ - a Bottom-up Convergent Approach for π-Extended Systems
Farinone, Marco; Kijewska, Monika; Cybińska, Joanna; Siczek, Milosz; Pawlicki, Miłosz; Chemical Communications  (2022) –; doi:10.1039/D2CC01801B

data_7130147
_publ_section_title
;
 B,N-doped PAHs from Tridentate &#x2018;Defects&#x2019; - a Bottom-up
 Convergent Approach for \p-Extended Systems
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01801B
_journal_year                    2022
_chemical_formula_moiety         'C29 H20 N4 O, C H2 Cl2'
_chemical_formula_sum            'C30 H22 Cl2 N4 O'
_chemical_formula_weight         525.41
_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-2018/1
_audit_update_record
;
2022-02-19 deposited with the CCDC.	2022-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.74(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.438(5)
_cell_length_b                   29.605(3)
_cell_length_c                   9.885(7)
_cell_measurement_reflns_used    1838
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.05
_cell_measurement_theta_min      5.36
_cell_volume                     2452(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1956
_diffrn_detector_type            Onyx
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur PX with Onyx CCD detector'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0944
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8913
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.497
_diffrn_reflns_theta_max         67.497
_diffrn_reflns_theta_min         2.985
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.640
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4372
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1346
_refine_ls_R_factor_gt           0.1087
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1291P)^2^+6.2223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2766
_refine_ls_wR_factor_ref         0.2956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3107
_reflns_number_total             4372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01801b2.cif
_cod_data_source_block           mf007a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7130147
_shelx_shelxl_version_number     2018/1
_oxdiff_exptl_absorpt_empirical_full_min 0.571
_oxdiff_exptl_absorpt_empirical_full_max 2.576
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              41294
_shelx_hkl_checksum              49482