Synthesis, Structure and Reactivity of a Borylene Cation [(NHSi)2B(CO)]+ Stabilized by Three Neutral Ligands.
Wang, Hao; Wu, Linlin; Lin, Zhenyang; Xie, Zuowei; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b08667

data_4126396
_publ_section_title
;
 Synthesis, Structure and Reactivity of a Borylene Cation [(NHSi)2B(CO)]+
 Stabilized by Three Neutral Ligands.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08667
_journal_year                    2017
_chemical_formula_sum            'C36 H64 B11 Cl2 Cu N4 O Si2'
_chemical_formula_weight         878.44
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 94.3906(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8320(8)
_cell_length_b                   19.0753(9)
_cell_length_c                   17.8224(9)
_cell_measurement_reflns_used    468
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     5705.5(5)
_computing_cell_refinement       'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_collection       'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_reduction        'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER D8VENTURE DIFFRACTOMETER'
_diffrn_measurement_method       'PHI & OMEGA SCAN'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.0517
_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       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            135203
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.292
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6498
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         10338
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0857
_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^)+(0.1740P)^2^+1.5257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2609
_refine_ls_wR_factor_ref         0.2901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6961
_reflns_number_total             10338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08667_si_003.cif
_cod_data_source_block           3
_cod_database_code               4126396
_shelx_estimated_absorpt_t_min   0.811
_shelx_estimated_absorpt_t_max   0.899
_shelxl_version_number           2014/6
_shelx_res_checksum              17133
_shelx_hkl_checksum              21041