Synthesis and Structural Characterization of Pentaarylboroles and Their Dianions
So, Cheuk-Wai; Watanabe, Daisuke; Wakamiya, Atsushi; Yamaguchi, Shigehiro; Organometallics 27 (2008) 3496–; doi:10.1021/om8002812

data_4071631
_publ_section_title
;
 Synthesis and Structural Characterization of Pentaarylboroles and Their
 Dianions
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3496
_journal_paper_doi               10.1021/om8002812
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C61 H81 B K2 N2 O4.5 Si'
_chemical_formula_weight         1031.38
_chemical_name_systematic
; 
1-(trimethylsilylphenyl)-2,3,4,5-tetraphenyl
borole dianion 
;
_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                80.90
_cell_angle_beta                 65.21
_cell_angle_gamma                63.44
_cell_formula_units_Z            2
_cell_length_a                   14.755
_cell_length_b                   14.738
_cell_length_c                   16.506
_cell_measurement_reflns_used    8050
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5050
_cell_measurement_theta_min      2.5458
_cell_volume                     2912.828
_computing_molecular_graphics    'ORTEP 3 for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type
;
Saturn70 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19749
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.9977
_exptl_absorpt_correction_T_min  0.9977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         10097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0723P)^2^+2.5529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                7922
_reflns_number_total             10097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8002812-file004.cif
_cod_data_source_block           comp6
_cod_original_cell_volume        2912.7
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C61 H81 B K2 N2 O4.50 Si'
_cod_database_code               4071631