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_7117788
_publ_section_title
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 Synthesis of a diboryl-N-heterocycle and its conversion to a bidentate
 cationic Lewis acid
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_journal_name_full               Chem.Commun.
_journal_page_first              14322
_journal_paper_doi               10.1039/C5cc06248A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'B C24 F20, C20 H32 B2 N2'
_chemical_formula_sum            'C44 H32 B3 F20 N2'
_chemical_formula_weight         1001.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2516(9)
_cell_length_b                   17.7060(9)
_cell_length_c                   27.4233(14)
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    149
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.42
_cell_volume                     8376.6(7)
_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 0.9999
_diffrn_measured_fraction_theta_max 0.9999
_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  0.0277
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            90800
_diffrn_reflns_theta_full        24.9991
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.81
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.5876
_exptl_crystal_density_meas      .
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             4043.7039
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.0959
_refine_diff_density_min         -0.4880
_refine_diff_density_rms         0.0896
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             11.2655
_refine_ls_goodness_of_fit_ref   1.0735
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    51
_refine_ls_number_parameters     621
_refine_ls_number_reflns         7379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0735
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+29.0718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.1942
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                6629
_reflns_number_total             7379
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5cc06248a2.cif
_cod_data_source_block           jf049_0ma
_cod_original_cell_volume        8376.6(8)
_cod_database_code               7117788
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C9(H9), C17(H17), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19a,H19b), C20(H20a,H20b), C10(H10a,H10b), C11(H11a,H11b), C14(H14a,
 H14b), C18(H18a,H18b), C16(H16a,H16b), C8(H8a,H8b), C7(H7a,H7b), C6(H6a,H6b),
 C12(H12a,H12b)
2.c Me refined with riding coordinates:
 C4(H4a,H4b,H4c)
2.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C2(H2), C3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'