Synthesis and Characterization of Terpyridine-Supported Boron Cations: Evidence for Pentacoordination at Boron
Gregory P. McGovern; Di Zhu; Adelia J. A. Aquino; Dragoslav Vidović; Michael Findlater; Inorganic Chemistry 52 (2013) 13865–13868; doi:10.1021/ic401486y

data_4336957
_publ_section_title
;
 Synthesis and Characterization of Terpyridine-Supported Boron Cations:
 Evidence for Pentacoordination at Boron
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13865
_journal_page_last               13868
_journal_paper_doi               10.1021/ic401486y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C21 H29 B Br N4 Si2, Br, C H2 Cl2'
_chemical_formula_sum            'C22 H31 B Br2 Cl2 N4 Si2'
_chemical_formula_weight         649.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.28(3)
_cell_angle_beta                 102.24(3)
_cell_angle_gamma                91.75(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8095(18)
_cell_length_b                   10.143(2)
_cell_length_c                   19.025(4)
_cell_measurement_temperature    153(2)
_cell_volume                     1618.2(6)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
'DENZO and Scalepack (Otwinoski and Minor, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.786
_diffrn_measured_fraction_theta_max 0.722
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0804
_diffrn_reflns_av_sigmaI/netI    0.1910
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7170
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    2.760
_exptl_absorpt_correction_T_max  0.7817
_exptl_absorpt_correction_T_min  0.6253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'DENZO and Scalepack (Otwinoski and Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       prism
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The SQUEEZED electron density of 61 e^-^/cell was accounted for as two
 molecules of CH~2~Cl~2~ solvent, at 40 e^-^ each.  This allows for one molecule
 of CH~2~Cl~2~per complex.  This solvent has been included in the final formula,
 formula weight, calculated density, \m and F(000).
;
_refine_diff_density_max         2.377
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.277
_refine_ls_R_factor_all          0.1882
_refine_ls_R_factor_gt           0.1199
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2829
_refine_ls_wR_factor_ref         0.3031
_reflns_number_gt                2544
_reflns_number_total             5510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401486y_si_002.cif
_cod_data_source_block           mfmf7s
_cod_database_code               4336957