Heavier Carbonyl Olefination: The Sila-Wittig Reaction.
Reiter, Dominik; Frisch, Philipp; Szilvási, Tibor; Inoue, Shigeyoshi; Journal of the American Chemical Society 141 (2019) 16991–16996; doi:10.1021/jacs.9b09379

data_4133719
_publ_section_title
;
 Heavier Carbonyl Olefination: The Sila-Wittig Reaction.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16991
_journal_page_last               16996
_journal_paper_doi               10.1021/jacs.9b09379
_journal_volume                  141
_journal_year                    2019
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C48 H79 N5 Si2'
_chemical_formula_sum            'C48 H79 N5 Si2'
_chemical_formula_weight         782.34
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.695(3)
_cell_length_b                   18.5885(19)
_cell_length_c                   25.738(2)
_cell_measurement_reflns_used    9307
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.6340
_cell_measurement_theta_min      2.4834
_cell_volume                     11336(2)
_computing_cell_refinement       'SAINT (Bruker, 2017)'
_computing_data_collection       'APEX III Control Software (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2017)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'
_computing_structure_refinement
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'Helios optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'IMS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            488979
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2, Bruker, 2016'
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_density_diffrn    0.917
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.253
_platon_squeeze_details
;
The unit cell contains 3 disordered molecules of toluene and n-hexane which were
treated as a diffuse contribution to the overall scattering without specific
atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         10380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0456P)^2^+6.2777P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                9550
_reflns_number_total             10380
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja9b09379_si_002.cif
_cod_data_source_block           compound_11
_cod_database_code               4133719
_shelx_res_checksum              64547
_shelx_hkl_checksum              62379
_shelx_fab_checksum              76102