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_4328488
_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 H10 B1 F30 N6 Tl1'
_chemical_formula_sum            'C45 H10 B F30 N6 Tl'
_chemical_formula_weight         1419.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.027(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5920(4)
_cell_length_b                   21.8080(5)
_cell_length_c                   11.1760(2)
_cell_measurement_reflns_used    22545
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.1506
_cell_measurement_theta_min      2.5981
_cell_measurement_wavelength     0.71073
_cell_volume                     5006.42(18)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, 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, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.0173372027
_diffrn_orient_matrix_UB_12      0.0310084302
_diffrn_orient_matrix_UB_13      -0.0049344102
_diffrn_orient_matrix_UB_21      0.0608556108
_diffrn_orient_matrix_UB_22      0.0092331605
_diffrn_orient_matrix_UB_23      0.0046097764
_diffrn_orient_matrix_UB_31      0.0063650646
_diffrn_orient_matrix_UB_32      -0.0033513012
_diffrn_orient_matrix_UB_33      -0.0338368084
_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  0.0317
_diffrn_reflns_av_unetI/netI     0.03
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            38754
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.379
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.27 (release 29-05-2008 CrysAlis171 .NET)
        (compiled May 29 2008,13:12:44)
        empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_description       plate
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.21
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         10217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+2.2377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.078
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                8102
_reflns_number_total             10217
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202125c_si_001_7.cif
_cod_data_source_block           Tl4
_cod_database_code               4328488