Facile Route to Quadruply Annulated Borepins.
Schickedanz, Kai; Radtke, Julian; Bolte, Michael; Lerner, Hans-Wolfram; Wagner, Matthias; Journal of the American Chemical Society 139 (2017) 2842–2851; doi:10.1021/jacs.7b00268

data_4125507
_publ_section_title
;
 Facile Route to Quadruply Annulated Borepins.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2842
_journal_page_last               2851
_journal_paper_doi               10.1021/jacs.7b00268
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C30 H21 B Br2, 0.5(C H Cl3)'
_chemical_formula_sum            'C30.5 H21.5 B Br2 Cl1.5'
_chemical_formula_weight         611.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.3271(5)
_cell_length_b                   8.32640(10)
_cell_length_c                   20.8885(3)
_cell_measurement_reflns_used    116918
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      1.95
_cell_volume                     5100.75(13)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            133329
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.950
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    3.354
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       needle
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.052
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5215
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0560P)^2^+14.0522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4930
_reflns_number_total             5215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00268_si_002.cif
_cod_data_source_block           wa2363
_cod_depositor_comments
'Adding full bibliography for 4125504--4125509.cif.'
_cod_original_cell_volume        5100.74(13)
_cod_original_formula_sum        'C30.50 H21.50 B Br2 Cl1.50'
_cod_database_code               4125507
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.599
_shelx_estimated_absorpt_t_max   0.906
_shelx_res_checksum              43421
_shelx_hkl_checksum              96504