Exhaustively Trichlorosilylated C<sub>1</sub> and C<sub>2</sub> Building Blocks: Beyond the Müller-Rochow Direct Process.
Georg, Isabelle; Teichmann, Julian; Bursch, Markus; Tillmann, Jan; Endeward, Burkhard; Bolte, Michael; Lerner, Hans-Wolfram; Grimme, Stefan; Wagner, Matthias; Journal of the American Chemical Society 140 (2018) 9696–9708; doi:10.1021/jacs.8b05950

data_4132737
_publ_section_title
;
 Exhaustively Trichlorosilylated C<sub>1</sub> and C<sub>2</sub> Building
 Blocks: Beyond the M\"uller-Rochow Direct Process.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9696
_journal_page_last               9708
_journal_paper_doi               10.1021/jacs.8b05950
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C Cl9 Si3, C16 H36 N'
_chemical_formula_sum            'C17 H36 Cl9 N Si3'
_chemical_formula_weight         657.79
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_Hall           'P -4n 2 3'
_space_group_name_H-M_alt        'P -4 3 n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5044(8)
_cell_length_b                   18.5044(8)
_cell_length_c                   18.5044(8)
_cell_measurement_reflns_used    10718
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.8
_cell_measurement_theta_min      1.6
_cell_volume                     6336.1(5)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16336
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.345
_diffrn_reflns_theta_min         1.556
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
; 
 Flack x determined using 597 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.06(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0486P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    0.903
_reflns_Friedel_fraction_max     0.890
_reflns_number_gt                1713
_reflns_number_total             2057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05950_si_002.cif
_cod_data_source_block           wa1715
_cod_original_cell_volume        6336.1(8)
_cod_database_code               4132737
_shelx_estimated_absorpt_t_min   0.898
_shelx_estimated_absorpt_t_max   0.922
_shelxl_version_number           2013-3
_shelx_res_checksum              67775
_shelx_hkl_checksum              80742