Synthesis of a diboryl-N-heterocycle and its conversion to a bidentate cationic Lewis acid
Jeffrey M. Farrell; Douglas W. Stephan; Chem.Commun. 51 (2015) 14322–; doi:10.1039/C5cc06248A

data_7117787
_publ_section_title
;
 Synthesis of a diboryl-N-heterocycle and its conversion to a bidentate
 cationic Lewis acid
;
_journal_name_full               Chem.Commun.
_journal_page_first              14322
_journal_paper_doi               10.1039/C5cc06248A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C20 H33 B2 I N2'
_chemical_formula_sum            'C20 H33 B2 I N2'
_chemical_formula_weight         450.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2015-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-21 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.364(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5093(5)
_cell_length_b                   7.7961(3)
_cell_length_c                   18.6255(6)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.28
_cell_volume                     2021.50(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      149.7
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40385
_diffrn_reflns_theta_full        24.9989
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.589
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0447 before and 0.0286 after correction.
The Ratio of minimum to maximum transmission is 0.9523.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.4786
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             918.6018
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.4034
_refine_diff_density_min         -0.2901
_refine_diff_density_rms         0.0522
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             12.8821
_refine_ls_goodness_of_fit_ref   1.0518
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     357
_refine_ls_number_reflns         3555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0518
_refine_ls_R_factor_all          0.0153
_refine_ls_R_factor_gt           0.0143
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+1.4274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0406
_refine_ls_wR_factor_ref         0.0412
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -17
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              -10
_reflns_number_gt                3414
_reflns_number_total             3555
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5cc06248a2.cif
_cod_data_source_block           jf052_0m
_cod_database_code               7117787
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'