Disilanes with Pentacoordinate Si Atoms by Carbon Dioxide Insertion into Aminodisilanes: Syntheses, Molecular Structures, and Dynamic Behavior.
Ryll, Christopher; Kraushaar, Konstantin; Wagler, Jörg; Brendler, Erica; Kroke, Edwin; ACS omega 7 (2022) 9527–9536; doi:10.1021/acsomega.1c06868

data_4519414
_publ_section_title
;
 Disilanes with Pentacoordinate Si Atoms by Carbon Dioxide Insertion into
 Aminodisilanes: Syntheses, Molecular Structures, and Dynamic Behavior.
;
_journal_issue                   11
_journal_name_full               'ACS omega'
_journal_page_first              9527
_journal_page_last               9536
_journal_paper_doi               10.1021/acsomega.1c06868
_journal_volume                  7
_journal_year                    2022
_chemical_formula_moiety         'C26 H46 N4 O8 Si2, 2(C H Cl3)'
_chemical_formula_sum            'C28 H48 Cl6 N4 O8 Si2'
_chemical_formula_weight         837.58
_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
_atom_sites_solution_primary     ShelXT
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.602(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3555(6)
_cell_length_b                   19.1906(8)
_cell_length_c                   10.8119(6)
_cell_measurement_reflns_used    25806
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.84
_cell_volume                     1940.38(18)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25149
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.839
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.9450
_exptl_absorpt_correction_T_min  0.8252
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XShape
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         4682
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0404P)^2^+0.6780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3821
_reflns_number_total             4682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c06868_si_002.cif
_cod_data_source_block           cr-p25d2-4cli_01
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4519414
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.931
_shelx_res_checksum              94885
_shelx_hkl_checksum              83249