Circumventing redox chemistry: synthesis of transition metal boryl complexes from a boryl nucleophile by decarbonylation.
Frank, René; Howell, James; Tirfoin, Rémi; Dange, Deepak; Jones, Cameron; Mingos, D Michael P; Aldridge, Simon; Journal of the American Chemical Society 136 (2014) 15730–15741; doi:10.1021/ja508979x

data_4122854
_publ_section_title
;
 Circumventing redox chemistry: synthesis of transition metal boryl
 complexes from a boryl nucleophile by decarbonylation.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15730
_journal_page_last               15741
_journal_paper_doi               10.1021/ja508979x
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C60 H88 B2 Br2 Mn2 N4 O2'
_chemical_formula_weight         1188.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.992(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4142(4)
_cell_length_b                   22.9367(7)
_cell_length_c                   13.8197(7)
_cell_measurement_temperature    123(2)
_cell_volume                     3157.0(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19551
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.707
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         6189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0418P)^2^+3.7149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                4752
_reflns_number_total             6189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja508979x_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4122854--4122863.cif.'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4122854