Direct access to a cAAC-supported dihydrodiborene and its dianion.
Arrowsmith, Merle; Mattock, James D.; Böhnke, Julian; Krummenacher, Ivo; Vargas, Alfredo; Braunschweig, Holger; Chemical communications (Cambridge, England) 54 (2018) 4669–4672; doi:10.1039/c8cc01580e

data_7121375
_publ_section_title
;
 Direct access to a cAAC-supported dihydrodiborene and its dianion.
;
_journal_issue                   37
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4669
_journal_page_last               4672
_journal_paper_doi               10.1039/c8cc01580e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '2 (C40 H56 B Cl K N O6), (squeezed solvent)'
_chemical_formula_sum            'C80 H112 B2 Cl2 K2 N2 O12'
_chemical_formula_weight         1464.43
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-02-21 deposited with the CCDC.
2018-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                112.102(2)
_cell_angle_beta                 90.824(2)
_cell_angle_gamma                110.440(2)
_cell_formula_units_Z            2
_cell_length_a                   14.7415(8)
_cell_length_b                   20.0443(13)
_cell_length_c                   22.6574(15)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.24
_cell_measurement_theta_min      2.66
_cell_volume                     5729.8(6)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014) '
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            101079
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.172
_diffrn_source
'rotating-anode X-ray tube or sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.849
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.118
_refine_diff_density_max         1.505
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0045(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         23362
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+15.8012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1923
_refine_ls_wR_factor_ref         0.2241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14012
_reflns_number_total             23362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01580e2.cif
_cod_data_source_block           triclin_a_sq_sq
_cod_depositor_comments
'Adding full bibliography for 7121372--7121375.cif.'
_cod_database_code               7121375
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.980
_exptl_absorpt_special_details
;The crystal was immersed in a film of perfluoropolyether oil, 
mounted on a a glass fiber and transferred to stream of cold nitrogen.
;
_shelx_res_checksum              75971
_shelx_fab_checksum              11880