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_4328487
_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         'C45 H28 B1 F12 N6 Tl1'
_chemical_formula_sum            'C45 H28 B F12 N6 Tl'
_chemical_formula_weight         1095.91
_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                104.709(3)
_cell_angle_beta                 96.815(6)
_cell_angle_gamma                100.048(5)
_cell_formula_units_Z            2
_cell_length_a                   11.2334(8)
_cell_length_b                   13.2250(11)
_cell_length_c                   15.366(2)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.2
_cell_measurement_theta_min      2.3
_cell_measurement_wavelength     0.71073
_cell_volume                     2142.1(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       \w-\f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            64621
_diffrn_reflns_theta_full        32.1
_diffrn_reflns_theta_max         32.1
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.863
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       plate
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         14857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.058
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                12371
_reflns_number_total             14857
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202125c_si_001_6.cif
_cod_data_source_block           Tl3
_cod_original_cell_volume        2142.0(4)
_cod_original_sg_symbol_H-M      'P - 1'
_cod_database_code               4328487