Thermal dehydrochlorination in the 4-fluoroaniline-trichloroborane system: identification of reactive intermediates involved in the formation of B,B',B''-trichloro-N,N',N''-tri((4-fluoro)phenyl)borazine.
Hahn, Jennifer; Krieg, Matthias; Keck, Constanze; Maichle-Mössmer, Cäcilia; Fink, Reinhold F.; Bettinger, Holger F.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 17304–17316; doi:10.1039/c8dt03954b

data_7048248
_publ_section_title
;
 Thermal dehydrochlorination in the 4-fluoroaniline-trichloroborane
 system: identification of reactive intermediates involved in the
 formation of B,B',B''-trichloro-N,N',N''-tri((4-fluoro)phenyl)borazine.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17304
_journal_page_last               17316
_journal_paper_doi               10.1039/c8dt03954b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C6 H6 B Cl3 F N'
_chemical_formula_weight         228.28
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-03-02 deposited with the CCDC.
2018-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2213(3)
_cell_length_b                   12.4120(3)
_cell_length_c                   6.7073(2)
_cell_measurement_reflns_used    4951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.446
_cell_volume                     934.18(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker COSMO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-13 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10743
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.306
_diffrn_reflns_theta_min         1.641
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  0.9590
_exptl_absorpt_correction_T_min  0.8400
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       needle
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 899 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.11(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2231
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0396P)^2^+0.1727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.766
_reflns_Friedel_fraction_full    0.950
_reflns_Friedel_fraction_max     0.911
_reflns_number_gt                2138
_reflns_number_total             2231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03954b2.cif
_cod_data_source_block           1a_mo_fr1
_cod_depositor_comments
'Adding full bibliography for 7048248--7048250.cif.'
_cod_database_code               7048248
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.959
_shelxl_version_number           2013-3
_shelx_res_checksum              26031