Magnesium-catalyzed hydrosilylation of α,β-unsaturated esters
Lampland, Nicole L.; Pindwal, Aradhana; Neal, Steven R.; Schlauderaff, Shealyn; Ellern, Arkady; Sadow, Aaron D.; Chem. Sci. 6 (2015) 6901–; doi:10.1039/C5SC02435H

data_1529471
_publ_section_title
;
 Magnesium-catalyzed hydrosilylation of \a,\b-unsaturated esters
;
_journal_issue                   12
_journal_name_full               'Chem. Sci.'
_journal_page_first              6901
_journal_paper_doi               10.1039/C5SC02435H
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C39 H30 B2 F15 Mg N3 O3, 2.5(C7 H8)'
_chemical_formula_sum            'C56.5 H50 B2 F15 Mg N3 O3'
_chemical_formula_weight         1149.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                86.434(3)
_cell_angle_beta                 88.133(3)
_cell_angle_gamma                69.802(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7916(18)
_cell_length_b                   13.460(2)
_cell_length_c                   18.239(3)
_cell_measurement_reflns_used    3354
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      22.3036
_cell_measurement_theta_min      2.1651
_cell_volume                     2711.3(7)
_computing_cell_refinement       'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_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       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15346
_diffrn_reflns_theta_full        24.81
_diffrn_reflns_theta_max         24.81
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1182
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
SQUEEZE (PLATON, A.Spek) was used to treat diffuse solvent and anion 
 contributions.  Total electron count found = 53/unit cell.  calculated for
 one toluene molecule (the only solvent for crystallization used) = 50/unit
 cell.  The intensive  properties (density, F(000), etc.) reflect these
 contributions.
;
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.433
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.730
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         9197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.730
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.2000P)^2^]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.2004
_reflns_number_gt                6299
_reflns_number_total             9197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02435h2.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 1529471.cif.'
_cod_original_formula_sum        'C56.50 H50 B2 F15 Mg N3 O3'
_cod_database_code               1529471