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_4126987
_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         'C53 H72 B2 N2 O3 W'
_chemical_formula_sum            'C53 H72 B2 N2 O3 W'
_chemical_formula_weight         990.59
_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_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.427(6)
_cell_length_b                   22.131(7)
_cell_length_c                   27.116(8)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.65
_cell_volume                     9858(6)
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (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      101(2)
_diffrn_detector                 'CMOS area detector (Photon 100)'
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0366
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            61691
_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         26.372
_diffrn_reflns_theta_min         2.154
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_exptl_absorpt_coefficient_mu    2.386
_exptl_absorpt_correction_T_max  0.4920
_exptl_absorpt_correction_T_min  0.3599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/4 (Bruker AXS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             4096
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.322
_exptl_crystal_size_min          0.258
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         10077
_refine_ls_number_restraints     360
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0138P)^2^+13.1002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8150
_reflns_number_total             10077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12394_si_004.cif
_cod_data_source_block           test_a
_cod_database_code               4126987
_shelx_estimated_absorpt_t_min   0.459
_shelx_estimated_absorpt_t_max   0.578
_shelxl_version_number           2014/6
_shelx_res_checksum              44339
_shelx_hkl_checksum              38813