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_7121373
_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         'C40 H56 B Cl K N O6, 4 (C7 H8)'
_chemical_formula_sum            'C68 H88 B Cl K N O6'
_chemical_formula_weight         1100.74
_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                98.287(2)
_cell_angle_beta                 92.396(2)
_cell_angle_gamma                109.232(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1241(8)
_cell_length_b                   14.4945(8)
_cell_length_c                   17.6107(10)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.22
_cell_volume                     3115.7(3)
_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 3888
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker Apex III (CCD)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0995
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43512
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.509
_diffrn_source
'rotating-anode X-ray tube or sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2014/4 (Bruker 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0076(14)
_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   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1318
_refine_ls_number_reflns         12401
_refine_ls_number_restraints     2432
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1828
_refine_ls_R_factor_gt           0.0881
_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^)+(0.1253P)^2^+5.3985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2217
_refine_ls_wR_factor_ref         0.2912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6275
_reflns_number_total             12401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01580e2.cif
_cod_data_source_block           final_a
_cod_depositor_comments
'Adding full bibliography for 7121372--7121375.cif.'
_cod_database_code               7121373
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.959
_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              56956