Synthesis of a bicyclic diborane by selective boron carbon bond formation
Holger Braunschweig; Alexander Damme; Thomas Kupfer; Chem.Commun. 49 (2013) 2774–; doi:10.1039/c3cc38789e

data_7109019
_publ_section_title
;
 Synthesis of a bicyclic diborane by selective boron carbon bond formation
;
_journal_name_full               Chem.Commun.
_journal_page_first              2774
_journal_paper_doi               10.1039/c3cc38789e
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C24 H36 B2 I N'
_chemical_formula_sum            'C24 H36 B2 I N'
_chemical_formula_weight         487.06
_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                95.40(3)
_cell_angle_beta                 90.39(3)
_cell_angle_gamma                104.22(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3238(17)
_cell_length_b                   8.5956(17)
_cell_length_c                   16.157(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1115.1(4)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2010.3 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4353
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    1.446
_exptl_absorpt_correction_T_max  0.158270
_exptl_absorpt_correction_T_min  0.121601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TwinAbs 2008/3 (Bruker 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0432P)^2^+0.6779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                4268
_reflns_number_total             4363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc38789e.txt
_cod_data_source_block           CCDC-912614
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7109019