Mild Synthesis of Diboryldiborenes by Diboration of B-B Triple Bonds
Brueckner, Tobias; Dewhurst, Rian David; Dellermann, Theresa; Müller, Marcel; Braunschweig, Holger; Chemical Science  (2019) –; doi:10.1039/C9SC02544H

data_1551353
_publ_section_title
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 Mild Synthesis of Diboryldiborenes by Diboration of B-B Triple Bonds
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02544H
_journal_year                    2019
_chemical_formula_moiety         'C58 H67 B4 N4 S4'
_chemical_formula_sum            'C58 H67 B4 N4 S4'
_chemical_formula_weight         991.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-11-29 deposited with the CCDC.    2019-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                106.073(17)
_cell_angle_beta                 100.060(18)
_cell_angle_gamma                94.42(3)
_cell_formula_units_Z            4
_cell_length_a                   12.532(4)
_cell_length_b                   18.541(5)
_cell_length_c                   26.605(5)
_cell_measurement_reflns_used    9156
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      2.26
_cell_volume                     5797(3)
_computing_cell_refinement       'Saint+ ver. V8.37A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.37A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CMOS area detector (Photon II)'
_diffrn_detector_area_resol_mean 7.5
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            141897
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.041
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_exptl_absorpt_coefficient_mu    0.203
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       block
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.222
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1323
_refine_ls_number_reflns         22818
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+1.4559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1437
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16790
_reflns_number_total             22818
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02544h2.cif
_cod_data_source_block           2b
_cod_depositor_comments
;

2022-11-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
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_cod_original_formula_sum            'C116 H134 B8 N8 S8'
_cod_original_formula_weight         1983.26
_cod_original_formula_moiety         'C116 H134 B8 N8 S8'
_cod_original_formula_units_Z            2
_cod_database_code               1551353
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.925
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              12440
_shelx_fab_checksum              58815