Complexation and Release of N-Heterocyclic Carbene-Aminoborylene Ligands from Group VI and VIII Metals.
Pranckevicius, Conor; Jimenéz-Halla, J Oscar C; Kirsch, Marius; Krummenacher, Ivo; Braunschweig, Holger; Journal of the American Chemical Society 140 (2018) 10524–10529; doi:10.1021/jacs.8b05398

data_4132669
_publ_section_title
;
 Complexation and Release of N-Heterocyclic Carbene-Aminoborylene Ligands
 from Group VI and VIII Metals.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10524
_journal_page_last               10529
_journal_paper_doi               10.1021/jacs.8b05398
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C26 H49 B Cl2 N2 Si2'
_chemical_formula_sum            'C26 H49 B Cl2 N2 Si2'
_chemical_formula_weight         527.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.894(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4346(4)
_cell_length_b                   24.9229(7)
_cell_length_c                   14.8706(6)
_cell_measurement_reflns_used    5354
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.95
_cell_measurement_theta_min      2.38
_cell_volume                     3444.6(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38295
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.214
_diffrn_reflns_theta_min         1.634
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
During the refinement of the structure, electron density 
peaks were located that were believed to be highly disordered 
tetrahydrofuran molecules. Attempts 
made to model the solvent molecule were not successful. 
The SQUEEZE option in PLATON (Spek, 2003) indicated there were two 
large solvent cavities of 343 A3 in the unit cell. 
In the final cycles of refinement, 
this contribution (83 electrons) to the electron density was 
removed from the observed  data. The density, the F(000) value, 
the molecular weight and the formula are given taking into 
account the results obtained with the SQUEEZE option PLATON 
(Spek, 2009).
;
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         7657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0433P)^2^+0.9205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5941
_reflns_number_total             7657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05398_si_002.cif
_cod_data_source_block           copr044_0m_sq
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4132669
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              45113
_platon_squeeze_void_probe_radius 1.20
_shelx_hkl_checksum              9660
_shelx_fab_checksum              9417