Utilisation of a lithium boryl as a reducing agent in low oxidation state group 15 chemistry: synthesis and characterisation of an amido-distibene and a boryl-dibismuthene
Deepak Dange; Amelia Davey; Joseph A. B. Abdalla; Simon Aldridge; Cameron Jones; Chem.Commun. 51 (2015) 7128–; doi:10.1039/C5cc01772F

data_7117003
_publ_section_title
;
 Utilisation of a lithium boryl as a reducing agent in low oxidation state
 group 15 chemistry: synthesis and characterisation of an amido-distibene
 and a boryl-dibismuthene
;
_journal_name_full               Chem.Commun.
_journal_page_first              7128
_journal_paper_doi               10.1039/C5cc01772F
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C51 H42 Bi Br2 N Si'
_chemical_formula_weight         1065.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                82.925(2)
_cell_angle_beta                 88.322(2)
_cell_angle_gamma                66.682(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3779(4)
_cell_length_b                   12.1720(4)
_cell_length_c                   18.3157(7)
_cell_measurement_temperature    123(2)
_cell_volume                     2108.00(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20733
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    6.143
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+2.0029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0655
_reflns_number_gt                7712
_reflns_number_total             8685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc01772f2.cif
_cod_data_source_block           compound1g
_cod_original_cell_volume        2108.00(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7117003