Synthesis and Functionalization of a 1,2-Bis(trimethylsilyl)-1,2-disilacyclohexene That Can Serve as a Unit of cis-1,2-Dialkyldisilene
Akasaka, N.; Tanaka, K.; Ishida, S.; Iwamoto, T.; Inorganics 6 (2018) 21–; doi:10.3390/inorganics6010021

data_1556587
_publ_section_title
;
 Synthesis and Functionalization of a
 1,2-Bis(trimethylsilyl)-1,2-disilacyclohexene That Can Serve as a Unit of
 cis-1,2-Dialkyldisilene
;
_journal_name_full               Inorganics
_journal_page_first              21
_journal_paper_doi               10.3390/inorganics6010021
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C33 H58 Si7'
_chemical_formula_sum            'C33 H58 Si7'
_chemical_formula_weight         651.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 91.2830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7493(8)
_cell_length_b                   9.0323(4)
_cell_length_c                   23.7624(10)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.20
_cell_measurement_theta_min      2.30
_cell_volume                     3808.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47339
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.148
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         7086
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+2.6595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6302
_reflns_number_total             7086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Cpd6_NA129a_a.cif
_cod_data_source_block           NA129a_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1556587
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.973
_shelxl_version_number           2014-3
_shelx_res_checksum              8690
_shelx_hkl_checksum              16022