Highly Fluorinated Aryl-Substituted Tris(indazolyl)borate Thallium Complexes: Diverse Regiochemistry at the B-N Bond
Wilfried-Solo Ojo; Kane Jacob; Emmanuelle Despagnet-Ayoub; Bianca K. Muñoz; Sergio Gonell; Laure Vendier; Viet-Hoang Nguyen; Michel Etienne; Inorganic Chemistry 51 (2012) 2893–2901; doi:10.1021/ic202125c

data_4328484
_publ_contact_author
;
Michel Etienne
;
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       Michel.Etienne@lcc-toulouse.fr
_publ_section_title
;
 Highly Fluorinated Aryl-Substituted Tris(indazolyl)borate Thallium
 Complexes: Diverse Regiochemistry at the B-N Bond
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2893
_journal_page_last               2901
_journal_paper_doi               10.1021/ic202125c
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C13 H F9 N2'
_chemical_formula_sum            'C13 H F9 N2'
_chemical_formula_weight         356.16
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                67.237(3)
_cell_angle_beta                 82.115(2)
_cell_angle_gamma                89.001(2)
_cell_formula_units_Z            2
_cell_length_a                   3.81860(10)
_cell_length_b                   12.3676(3)
_cell_length_c                   13.7752(4)
_cell_measurement_reflns_used    8502
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.17
_cell_measurement_theta_min      3.5686
_cell_measurement_wavelength     0.71073
_cell_volume                     593.77(3)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.011
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11765
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.58
_exptl_absorpt_coefficient_mu    0.22
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
        empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2253
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.14
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.1159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.081
_refine_ls_wR_factor_ref         0.083
_reflns_number_gt                1902
_reflns_number_total             2253
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202125c_si_001_3.cif
_cod_data_source_block           2
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_database_code               4328484