Computational, Mechanistic, and Experimental Insights into Regioselective Catalytic C-C Bond Activation in Linear 1-Aza-[3]triphenylene.
Ulč, Jan; Asanuma, Yuya; Moss, Robert; Manca, Gabriele; Císařová, Ivana; Kotora, Martin; ACS omega 7 (2022) 8665–8674; doi:10.1021/acsomega.1c06664

data_4519396
_publ_section_title
;
 Computational, Mechanistic, and Experimental Insights into Regioselective
 Catalytic C-C Bond Activation in Linear 1-Aza-[3]triphenylene.
;
_journal_issue                   10
_journal_name_full               'ACS omega'
_journal_page_first              8665
_journal_page_last               8674
_journal_paper_doi               10.1021/acsomega.1c06664
_journal_volume                  7
_journal_year                    2022
_chemical_formula_moiety         'C51 H45 N Si2, C H2 Cl2'
_chemical_formula_sum            'C52 H47 Cl2 N Si2'
_chemical_formula_weight         812.98
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 94.273(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2706(3)
_cell_length_b                   34.0842(13)
_cell_length_c                   15.5666(5)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      70.1038
_cell_measurement_theta_min      2.5927
_cell_volume                     4376.0(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.9'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios Cu  multilayer optic'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            50875
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.097
_diffrn_reflns_theta_min         2.593
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.130
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       needle
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.594
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0286P)^2^+8.8125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7035
_reflns_number_total             8269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c06664_si_002.cif
_cod_data_source_block           cu_ju_rm1_kotora
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4519396
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.364
_shelx_estimated_absorpt_t_max   0.878
_shelx_res_checksum              99071
_shelx_hkl_checksum              5760