Azaacenodibenzosuberones.
Brosius, Victor; Müller, Matthias; Borstelmann, Jan; Rominger, Frank; Freudenberg, Jan; Bunz, Uwe H. F.; The Journal of organic chemistry  (2019) –; doi:10.1021/acs.joc.9b02756

data_4036086
_publ_section_title
;
 Azaacenodibenzosuberones.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b02756
_journal_year                    2019
_chemical_formula_sum            'C49 H54 Cl3 N4 O Si2'
_chemical_formula_weight         877.49
_chemical_name_common            '3d in manuscript'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 95.694(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0785(5)
_cell_length_b                   32.5959(9)
_cell_length_c                   7.7799(2)
_cell_measurement_reflns_used    23048
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      69.80
_cell_measurement_theta_min      2.46
_cell_volume                     4562.0(2)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.144.0 (STOE, 2018)'
_computing_data_reduction        'X-Area Integrate 1.73.0.0 (STOE, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'STOE Stadivari'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            25286
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.819
_diffrn_reflns_theta_min         2.711
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    2.639
_exptl_absorpt_correction_T_max  1.342
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'STOE X-AREA LANA'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       plate
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         8302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+0.7938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5761
_reflns_number_total             8302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02756_si_002.cif
_cod_data_source_block           vb14_sq
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4036086
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.564
_shelx_estimated_absorpt_t_max   0.949
_exptl_absorpt_special_details   'X-Area LANA 1.70.0.0 (STOE, 2017)'
_shelx_res_checksum              28017
_shelx_hkl_checksum              86479
_shelx_fab_checksum              38018