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_4131782
_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         'C43 H75 N5 O Si5'
_chemical_formula_sum            'C43 H75 N5 O Si5'
_chemical_formula_weight         818.53
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                103.477(1)
_cell_angle_beta                 99.622(1)
_cell_angle_gamma                94.491(1)
_cell_formula_units_Z            4
_cell_length_a                   12.4388(5)
_cell_length_b                   20.3429(7)
_cell_length_c                   20.7659(8)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.4829
_cell_measurement_theta_min      2.3891
_cell_volume                     5000.2(3)
_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  0.0682
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            93632
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.133
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1095
_refine_ls_number_reflns         17649
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0327P)^2^+5.0730P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                13203
_reflns_number_total             17649
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja7b10634_si_002.cif
_cod_data_source_block           6
_cod_database_code               4131782
_shelx_res_checksum              23828
_shelx_hkl_checksum              45579