Synthesis and Characterization of a Boron-Nitrogen-Boron Zigzag-Edged Benzo[fg]tetracene Motif.
Fingerle, Michael; Maichle-Mössmer, Cäcilia; Schundelmeier, Simon; Speiser, Bernd; Bettinger, Holger F.; Organic letters 19 (2017) 4428–4431; doi:10.1021/acs.orglett.7b01873

data_1546789
_publ_section_title
;
 Synthesis and Characterization of a Boron-Nitrogen-Boron Zigzag-Edged
 Benzo[fg]tetracene Motif.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4428
_journal_page_last               4431
_journal_paper_doi               10.1021/acs.orglett.7b01873
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C40 H41 B2 N'
_chemical_formula_weight         557.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 115.5680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8877(2)
_cell_length_b                   24.3685(4)
_cell_length_c                   11.9282(2)
_cell_measurement_reflns_used    192
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.57
_cell_measurement_theta_min      1.895
_cell_volume                     3117.05(9)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Apex3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5,SHELXS-13 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Smart APEX II '
_diffrn_measurement_method       omega/phi-scans
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            61660
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.238
_diffrn_reflns_theta_min         1.671
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       column
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         16724
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.3284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                15029
_reflns_number_total             16724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b01873_si_002.cif
_cod_data_source_block           MFB2_0m
_cod_depositor_comments          'Adding full bibliography for 1546789.cif.'
_cod_database_code               1546789
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.971
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              4474
_shelx_hkl_checksum              23422