#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:12:02 +0100 (mar 22 de mar de 2016) $
#$Revision: 178940 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/69/4116968.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4116968
loop_
_publ_author_name
'Norbert W. Mitzel'
'Alexander J. Blake'
'David W. H. Rankin'
_publ_section_title
;
 β-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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0335P)²+0.7745P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Si 0.0383(5) 0.0383(5) 0.0262(5) 0.000 0.000 0.000
O 0.0480(8) 0.0361(7) 0.0373(6) -0.0052(5) 0.0116(5) -0.0032(5)
C1 0.0478(11) 0.0343(9) 0.0350(9) -0.0040(7) 0.0081(7) -0.0027(8)
C2 0.081(2) 0.0506(12) 0.0370(10) -0.0040(9) 0.0078(10) 0.0075(11)
C3 0.0623(14) 0.0496(13) 0.0535(12) -0.0022(10) -0.0028(10) 0.0077(10)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Si Si 0.0000 0.2500 0.1250 0.0343(4) Uani 1 d S
O O 0.16738(14) 0.22454(13) 0.08975(4) 0.0405(5) Uani 1 d .
C1 C 0.2158(2) 0.0705(2) 0.06403(6) 0.0391(5) Uani 1 d .
H1 H 0.1299(22) -0.0119(21) 0.0701(7) 0.040(4) Uiso 1 d .
C2 C 0.2324(3) 0.1012(3) 0.00397(7) 0.0563(6) Uani 1 d .
H21 H 0.3210(29) 0.1816(28) -0.0014(9) 0.070(6) Uiso 1 d .
H22 H 0.1280(30) 0.1469(28) -0.0113(8) 0.074(7) Uiso 1 d .
H23 H 0.2582(25) -0.0027(28) -0.0144(9) 0.063(6) Uiso 1 d .
C3 C 0.3740(3) 0.0110(3) 0.08971(9) 0.0551(6) Uani 1 d .
H31 H 0.4129(25) -0.0974(29) 0.0731(8) 0.068(6) Uiso 1 d .
H32 H 0.3606(27) -0.0059(26) 0.1283(11) 0.077(7) Uiso 1 d .
H33 H 0.4614(31) 0.0907(32) 0.0841(9) 0.082(8) Uiso 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O Si O 114.91(8) 12_666 15 y
O Si O 106.82(4) 12_666 . y
O Si O 106.82(4) 15 . ?
O Si O 106.82(4) 12_666 6_454 ?
O Si O 106.82(4) 15 6_454 ?
O Si O 114.91(8) . 6_454 ?
C1 O Si 124.68(10) . . y
O C1 C3 108.47(14) . . y
O C1 C2 108.31(14) . . y
C3 C1 C2 113.1(2) . . y
O C1 H1 109.0(9) . . y
C3 C1 H1 108.7(10) . . y
C2 C1 H1 109.2(10) . . y
C1 C2 H21 108.0(13) . . y
C1 C2 H22 111.0(12) . . y
H21 C2 H22 108.9(18) . . ?
C1 C2 H23 109.6(12) . . y
H21 C2 H23 110.6(17) . . ?
H22 C2 H23 108.9(17) . . ?
C1 C3 H31 111.5(12) . . y
C1 C3 H32 111.4(13) . . y
H31 C3 H32 108.2(17) . . ?
C1 C3 H33 110.3(14) . . y
H31 C3 H33 106.8(17) . . ?
H32 C3 H33 108.4(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si O 1.6152(10) 12_666 y
Si O 1.6152(10) 15 ?
Si O 1.6152(10) . ?
Si O 1.6152(10) 6_454 ?
O C1 1.445(2) . y
C1 C3 1.499(3) . y
C1 C2 1.507(2) . y
C1 H1 0.97(2) . y
C2 H21 0.97(2) . y
C2 H22 0.99(2) . y
C2 H23 0.97(2) . y
C3 H31 1.01(2) . y
C3 H32 0.97(3) . y
C3 H33 0.96(3) . y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_publ_flag
O Si O C1 162.75(13) 12_666 y
O Si O C1 39.30(9) 15 y
O Si O C1 -78.97(11) 6_454 y
Si O C1 C3 -115.9(2) . y
Si O C1 C2 121.07(15) . y
