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_7130154
_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
'Br4 Zn, 2(O4 Cl), C116 H72 B4 N16 O2, 0.45(H2 O), 0.583(C H4 O), 3.5(C7 H8)'
_chemical_formula_sum            'C141.09 H103.24 B4 Br4 Cl2 N16 O11.03 Zn'
_chemical_formula_weight         2698.36
_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   mixed
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2022-05-14 deposited with the CCDC.	2022-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                73.04(2)
_cell_angle_beta                 79.04(2)
_cell_angle_gamma                82.640(10)
_cell_formula_units_Z            2
_cell_length_a                   16.853(4)
_cell_length_b                   17.842(3)
_cell_length_c                   22.270(5)
_cell_measurement_reflns_used    20725
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.20
_cell_measurement_theta_min      3.49
_cell_volume                     6269(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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy DW system with HyPix-Arc 150 detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            84401
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.027
_diffrn_reflns_theta_min         3.529
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.712
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             2748
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.267
_refine_diff_density_min         -2.111
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.334
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1648
_refine_ls_number_reflns         24149
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.331
_refine_ls_R_factor_all          0.1788
_refine_ls_R_factor_gt           0.1345
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         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          0.3566
_refine_ls_wR_factor_ref         0.3852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15559
_reflns_number_total             24149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01801b2.cif
_cod_data_source_block           MF015_CU_100KA
_cod_database_code               7130154
_shelx_shelxl_version_number     2018/1
_oxdiff_exptl_absorpt_empirical_full_min 0.437
_oxdiff_exptl_absorpt_empirical_full_max 1.731
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              37429
_shelx_hkl_checksum              12782