Magnesium-catalyzed hydroboration of esters: evidence for a new zwitterionic mechanism
Mukherjee, Debabrata; Ellern, Arkady; Sadow, Aaron D.; Chemical Science 5 (2014) 959–; doi:10.1039/c3sc52793j

data_1513684
_publ_section_title
;
 Magnesium-catalyzed hydroboration of esters: evidence for a new
 zwitterionic mechanism
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              959
_journal_paper_doi               10.1039/c3sc52793j
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         '(C46 H68 B2 Mg2 N6 O8) (C6 D6)'
_chemical_formula_sum            'C52 H74 B2 Mg2 N6 O8'
_chemical_formula_weight         981.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX2 v2012.2-0'
_cell_angle_alpha                90
_cell_angle_beta                 99.963(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4348(11)
_cell_length_b                   19.441(2)
_cell_length_c                   14.2620(15)
_cell_measurement_temperature    173.(2)
_cell_volume                     2849.6(5)
_computing_cell_refinement       'SAINT V7.66A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 Suite (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.66A (Bruker AXS, 2009)'
_computing_molecular_graphics    'XSHELL (Bruker AXS, 2007)'
_computing_publication_material  'APEX2 Suite (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  ' BRUKER APEX2 CCD Diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22855
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
Amount of electrons squeezed  from the cell is in  good
accord with one diffused benzene-D6 in a void per one
cluster. 42 electrons were added to the final refinement
to obtain true metric outputs 
;
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5030
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.2452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                3721
_reflns_number_total             5030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52793j.txt
_cod_data_source_block           ToMMgOEt
_cod_database_code               1513684