β-Donor Bonds in SiON Units: An Inherent Structure- Determining Property Leading to (4 + 4)-Coordination in Tetrakis-(N,N-dimethylhydroxylamido)silane
Norbert W. Mitzel; Alexander J. Blake; David W. H. Rankin; Journal of the American Chemical Society 119 (1997) 4143–4148; doi:10.1021/ja9640004

data_4116968
_publ_section_title
;
 \b-Donor Bonds in SiON Units: An Inherent Structure- Determining Property
 Leading to (4 + 4)-Coordination in
 Tetrakis-(N,N-dimethylhydroxylamido)silane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4143
_journal_page_last               4148
_journal_paper_doi               10.1021/ja9640004
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C12 H28 O4 Si'
_chemical_formula_weight         264.43
_chemical_melting_point          249
_chemical_name_systematic
; 
Tetraisopropoxysilane 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0422(5)
_cell_length_b                   8.0422(5)
_cell_length_c                   24.653(2)
_cell_measurement_reflns_used    88
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      20.0
_cell_volume                     1594.48(19)
_computing_cell_refinement       'DIF4 (Stoe & Cie, 1990a)'
_computing_data_collection       'DIF4 (Stoe & Cie, 1990a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1990b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1992)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1992)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle diffractometer'
_diffrn_measurement_method       'omega-theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            2226
_diffrn_reflns_theta_max         60.05
_diffrn_reflns_theta_min         5.79
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.325
_exptl_absorpt_correction_T_max  0.330
_exptl_absorpt_correction_T_min  0.245
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       Cylinder
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.60
_refine_diff_density_max         0.098
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.030
_refine_ls_extinction_coef       0.0179(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.102
_refine_ls_goodness_of_fit_obs   1.121
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_restrained_S_obs      1.121
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_obs          0.0314
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.7745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0827
_refine_ls_wR_factor_obs         0.0782
_reflns_number_observed          555
_reflns_number_total             593
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9640004_2.cif
_cod_data_source_block           sioipr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.7745P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.7745P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1594.4(3)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4116968