Half-Sandwich Complexes of an Extremely Electron-Donating, Redox-Active η6-Diborabenzene Ligand.
Böhnke, Julian; Braunschweig, Holger; Jiménez-Halla, J Oscar C; Krummenacher, Ivo; Stennett, Tom E.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b12394

data_4126988
_publ_section_title
;
 Half-Sandwich Complexes of an Extremely Electron-Donating, Redox-Active
 \h6-Diborabenzene Ligand.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b12394
_journal_year                    2017
_chemical_formula_moiety         'C122 H176 B4 Li2 N4 O10 W2'
_chemical_formula_sum            'C122 H176 B4 Li2 N4 O10 W2'
_chemical_formula_weight         2283.48
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                74.006(3)
_cell_angle_beta                 88.671(2)
_cell_angle_gamma                77.596(2)
_cell_formula_units_Z            1
_cell_length_a                   10.4746(5)
_cell_length_b                   14.3447(9)
_cell_length_c                   20.4846(13)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      2.20
_cell_volume                     2887.6(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-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_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  0.1145
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            97584
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.992
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_exptl_absorpt_coefficient_mu    2.048
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             1190
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.964
_refine_diff_density_min         -3.173
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         11366
_refine_ls_number_restraints     242
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+1.0310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9603
_reflns_number_total             11366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12394_si_005.cif
_cod_data_source_block           test_a
_cod_database_code               4126988
_shelx_estimated_absorpt_t_min   0.678
_shelx_estimated_absorpt_t_max   0.921
_shelxl_version_number           2014/6
_shelx_res_checksum              54347
_shelx_hkl_checksum              55802