Boryl-assisted hydrogenolysis of a nickel-methyl bond
Natalia Curado; Celia Maya; Joaquin Lopez-Serrano; Amor Rodriguez; Chem.Commun. 50 (2014) 15718–; doi:10.1039/C4cc07616H

data_7116093
_publ_section_title
;
 Boryl-assisted hydrogenolysis of a nickel-methyl bond
;
_journal_name_full               Chem.Commun.
_journal_page_first              15718
_journal_paper_doi               10.1039/C4cc07616H
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C24 H44 B Br N2 Ni P2'
_chemical_formula_weight         571.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.7353(3)
_cell_length_b                   14.3656(4)
_cell_length_c                   32.1047(9)
_cell_measurement_reflns_used    8703
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.45
_cell_measurement_theta_min      2.33
_cell_volume                     5412.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0718
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            54490
_diffrn_reflns_theta_full        32.86
_diffrn_reflns_theta_max         32.86
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    2.326
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
 X-ray Solutions, Madison, Wisconsin, USA.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2400
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.506
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         10054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+2.3089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                7677
_reflns_number_total             10054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc07616h2.cif
_cod_data_source_block           aro0213a
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7116093