DMAP-stabilized bis(silyl)silylenes as versatile synthons for organosilicon compounds
Holzner, Richard; Reiter, Dominik; Frisch, Philipp; Inoue, Shigeyoshi; RSC Advances 10 (2020) 3402–3406; doi:10.1039/C9RA10628F

data_7239804
_publ_section_title
;
 DMAP-stabilized bis(silyl)silylenes as versatile synthons for
 organosilicon compounds
;
_journal_issue                   6
_journal_name_full               'RSC Advances'
_journal_page_first              3402
_journal_page_last               3406
_journal_paper_doi               10.1039/C9RA10628F
_journal_volume                  10
_journal_year                    2020
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C31 H73 N3 Si7'
_chemical_formula_sum            'C31 H73 N3 Si7'
_chemical_formula_weight         684.55
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2019-11-25 deposited with the CCDC.	2020-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                97.728(17)
_cell_angle_beta                 92.844(18)
_cell_angle_gamma                104.175(19)
_cell_formula_units_Z            2
_cell_length_a                   11.515(9)
_cell_length_b                   11.940(9)
_cell_length_c                   16.100(7)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.6177
_cell_measurement_theta_min      2.4954
_cell_volume                     2119(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            89033
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2, Bruker, 2016'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             756
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0445P)^2^+1.7142P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                7180
_reflns_number_total             7757
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c9ra10628f2.cif
_cod_data_source_block           Compound_7a
_cod_depositor_comments
'Adding full bibliography for 7239801--7239804.cif.'
_cod_database_code               7239804
_shelx_res_checksum              2393