Silicon and Oxygen's Bond of Affection: An Acyclic Three-Coordinate Silanone and Its Transformation to an Iminosiloxysilylene.
Wendel, Daniel; Reiter, Dominik; Porzelt, Amelie; Altmann, Philipp J.; Inoue, Shigeyoshi; Rieger, Bernhard; Journal of the American Chemical Society 139 (2017) 17193–17198; doi:10.1021/jacs.7b10634

data_4131779
_publ_section_title
;
 Silicon and Oxygen's Bond of Affection: An Acyclic Three-Coordinate
 Silanone and Its Transformation to an Iminosiloxysilylene.
;
_journal_issue                   47
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17193
_journal_page_last               17198
_journal_paper_doi               10.1021/jacs.7b10634
_journal_volume                  139
_journal_year                    2017
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C38 H66 N4 O Si5'
_chemical_formula_sum            'C38 H66 N4 O Si5'
_chemical_formula_weight         735.40
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 97.371(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3704(11)
_cell_length_b                   33.835(3)
_cell_length_c                   12.9525(12)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.9435
_cell_measurement_theta_min      2.3175
_cell_volume                     4507.2(8)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            48889
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.133
_refine_diff_density_max         1.312
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         7974
_refine_ls_number_restraints     682
_refine_ls_restrained_S_all      1.302
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0941
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.1137P)^2^+6.2488P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2488
_refine_ls_wR_factor_ref         0.2777
_reflns_number_gt                5222
_reflns_number_total             7974
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja7b10634_si_002.cif
_cod_data_source_block           2a
_cod_original_cell_volume        4507.3(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4131779
_shelx_res_checksum              20621
_shelx_hkl_checksum              30587