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_4519412
_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         'C22 H38 N4 O8 Si2, 2(C H Cl3)'
_chemical_formula_sum            'C24 H40 Cl6 N4 O8 Si2'
_chemical_formula_weight         781.48
_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   geom
_atom_sites_solution_primary     ShelXT
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                86.509(2)
_cell_angle_beta                 75.909(2)
_cell_angle_gamma                86.201(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7730(3)
_cell_length_b                   11.6396(3)
_cell_length_c                   16.0521(5)
_cell_measurement_reflns_used    34171
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      1.76
_cell_volume                     1765.26(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0195
_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       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32078
_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         27.997
_diffrn_reflns_theta_min         1.755
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.8941
_exptl_absorpt_correction_T_min  0.8026
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XShape
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       piece
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.0097(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         8513
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0415P)^2^+0.7739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7359
_reflns_number_total             8513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c06868_si_002.cif
_cod_data_source_block           cr-p1d2-1b_01
_cod_database_code               4519412
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.732
_shelx_estimated_absorpt_t_max   0.817
_shelx_res_checksum              76508
_shelx_hkl_checksum              33999