Organosilicon Radicals with Si-H and Si-Me Bonds from Commodity Precursors.
Kundu, Subrata; Samuel, Prinson P.; Sinhababu, Soumen; Luebben, Anna V.; Dittrich, Birger; Andrada, Diego M.; Frenking, Gernot; Stückl, A Claudia; Schwederski, Brigitte; Paretzki, Alexa; Kaim, Wolfgang; Roesky, Herbert W.; Journal of the American Chemical Society 139 (2017) 11028–11031; doi:10.1021/jacs.7b06610

data_4131535
_publ_section_title
;
 Organosilicon Radicals with Si-H and Si-Me Bonds from Commodity
 Precursors.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11028
_journal_page_last               11031
_journal_paper_doi               10.1021/jacs.7b06610
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C80 H128 N4 Si2'
_chemical_formula_weight         1202.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 100.27(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.125(4)
_cell_length_b                   9.556(3)
_cell_length_c                   23.278(6)
_cell_measurement_reflns_used    92126
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      1.09
_cell_volume                     7469(3)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'SHELXLE (Huebschle, 2011)'
_computing_publication_material  'enCIFer 1.5.1, CCDC, 2015'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Microdiffractometer at the SLS'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6358
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            114273
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        22.425
_diffrn_reflns_theta_max         25.077
_diffrn_reflns_theta_min         1.085
_diffrn_source                   'monochromated X-rays beamline X10SA@SLS'
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6978
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2016/2, multi-scan. (G. M. Sheldrick, 2016)
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.034
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         9228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0648P)^2^+3.8633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1070
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8870
_reflns_number_total             9228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06610_si_002.cif
_cod_data_source_block           skr219
_cod_original_cell_volume        7470(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4131535
_shelxl_version_number           2014/6
_shelx_res_checksum              19165
_shelx_hkl_checksum              13284