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_4132738
_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         '2(C16 H36 N), C2 Cl12 Si4'
_chemical_formula_sum            'C34 H72 Cl12 N2 Si4'
_chemical_formula_weight         1046.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                85.921(4)
_cell_angle_beta                 85.777(4)
_cell_angle_gamma                88.686(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4327(6)
_cell_length_b                   11.8063(6)
_cell_length_c                   19.5139(9)
_cell_measurement_reflns_used    68050
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      3.15
_cell_volume                     2619.7(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.991
_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  0.0555
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            69365
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.185
_diffrn_reflns_theta_min         3.266
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         10415
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0585
_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^+4.7391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8570
_reflns_number_total             10415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05950_si_002.cif
_cod_data_source_block           wa1790
_cod_database_code               4132738
_shelx_estimated_absorpt_t_min   0.773
_shelx_estimated_absorpt_t_max   0.915
_shelxl_version_number           2013-3
_shelx_res_checksum              63003
_shelx_hkl_checksum              66349