Magnesium hydride alkene insertion and catalytic hydrosilylation
García, Lucía; Dinoi, Chiara; Mahon, Mary F.; Laurent, Maron; Hill, Michael; Chemical Science  (2019) –; doi:10.1039/C9SC02056J

data_1552121
_publ_section_title
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 Magnesium hydride alkene insertion and catalytic hydrosilylation&#x00A0;
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02056J
_journal_year                    2019
_chemical_formula_moiety         'C36 H52 Mg N2'
_chemical_formula_sum            'C36 H52 Mg N2'
_chemical_formula_weight         537.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-01-17
_audit_creation_method           'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_audit_update_record
;
2019-04-25 deposited with the CCDC.    2019-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7502(3)
_cell_length_b                   20.6951(4)
_cell_length_c                   8.5719(2)
_cell_measurement_reflns_used    8105
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.2740
_cell_measurement_theta_min      4.2700
_cell_volume                     3326.22(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 8.1150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            28832
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.360
_diffrn_reflns_theta_min         4.273
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3443
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+0.8354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2753
_reflns_number_total             3443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02056j2.cif
_cod_data_source_block           s19msh6-Compound-15
_cod_database_code               1552121
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16-H16
 0.98 with sigma of 0.005
 C13-C14 \\sim C13-C14A
 with sigma of 0.02
 C13-C15 \\sim C13-C15A
 with sigma of 0.02
3. Others
 Fixed Sof: H13(0.5) H13A(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C15(0.5)
 H15A(0.5) H15B(0.5) H15C(0.5) C17(0.5) H17(0.5) C18(0.5) H18A(0.5) H18B(0.5)
 C19(0.5) H19A(0.5) H19B(0.5) C20(0.5) H20(0.5) C21(0.5) H21A(0.5) H21B(0.5)
 C22(0.5) H22A(0.5) H22B(0.5) C14A(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C15A(0.5)
 H15D(0.5) H15E(0.5) H15F(0.5)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C13(H13A), C17(H17), C20(H20)
4.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8)
4.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C14A(H14D,H14E,H14F), C15A(H15D,H15E,H15F)
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