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_4519410
_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         'C18 H38 N4 O8 Si2, C4 H8 O'
_chemical_formula_sum            'C22 H46 N4 O9 Si2'
_chemical_formula_weight         566.81
_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
_atom_sites_solution_primary     ShelXT
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                72.610(5)
_cell_angle_beta                 89.884(5)
_cell_angle_gamma                68.752(5)
_cell_formula_units_Z            2
_cell_length_a                   10.2419(7)
_cell_length_b                   11.9781(8)
_cell_length_c                   13.8119(8)
_cell_measurement_reflns_used    24109
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.80
_cell_volume                     1496.25(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      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0217
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21361
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.800
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.9864
_exptl_absorpt_correction_T_min  0.9193
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XShape
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       plate
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         7219
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0509P)^2^+0.6016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6242
_reflns_number_total             7219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c06868_si_002.cif
_cod_data_source_block           cr-kk268_02
_cod_original_cell_volume        1496.26(18)
_cod_database_code               4519410
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.905
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              25434
_shelx_hkl_checksum              93076