#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:58:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179272 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/92/4319270.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_4319270
loop_
_publ_author_name
'Vadapalli Chandrasekhar'
'Selvarajan Nagendran'
'Ramamoorthy Boomishankar'
'Raymond J. Butcher'
_publ_section_title
;
 Effect of Sterically Hindered Ligands on the Solid-State Structures of
 Organosilanediols Containing Si-N Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              940
_journal_page_last               945
_journal_paper_doi               10.1021/ic000487c
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C12 H23 N O2 Si2'
_chemical_formula_weight         269.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.759(9)
_cell_angle_beta                 101.022(14)
_cell_angle_gamma                94.454(13)
_cell_formula_units_Z            4
_cell_length_a                   10.496(2)
_cell_length_b                   11.4245(18)
_cell_length_c                   14.129(3)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9.97
_cell_measurement_theta_min      2.09
_cell_volume                     1616.0(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.746
_diffrn_measured_fraction_theta_max 0.746
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4594
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.10
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       thick_needle
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.0024(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.171
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0453P)²+1.0630P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                2983
_reflns_number_total             4254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000487c_1.cif
_cod_data_source_block           vc13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1616.1(5)
_cod_database_code               4319270
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si11 Si 0.03604(11) 0.48402(9) 0.16806(7) 0.0399(3) Uani 1 1 d . . .
Si12 Si 0.13119(13) 0.23406(10) 0.14964(8) 0.0567(4) Uani 1 1 d . . .
Si21 Si -0.44070(11) 0.59425(9) 0.17650(7) 0.0432(4) Uani 1 1 d . . .
Si22 Si -0.52809(13) 0.83967(10) 0.15526(9) 0.0609(4) Uani 1 1 d . . .
O11 O 0.1524(3) 0.5024(3) 0.1086(2) 0.0507(9) Uani 1 1 d . . .
H11 H 0.142(5) 0.513(5) 0.066(4) 0.09(2) Uiso 1 1 d . . .
O12 O -0.0999(3) 0.4799(3) 0.08669(19) 0.0517(8) Uani 1 1 d . . .
H12 H -0.163(5) 0.509(4) 0.105(3) 0.08(2) Uiso 1 1 d . . .
O21 O -0.5802(4) 0.5352(2) 0.1031(2) 0.0512(10) Uani 1 1 d . . .
H21 H -0.646(4) 0.533(3) 0.116(3) 0.033(14) Uiso 1 1 d . . .
O22 O -0.3379(3) 0.5705(3) 0.1024(2) 0.0586(10) Uani 1 1 d . . .
H22 H -0.363(5) 0.551(4) 0.054(3) 0.060(17) Uiso 1 1 d . . .
N1 N 0.0543(3) 0.3518(2) 0.20624(18) 0.0402(8) Uani 1 1 d . . .
N2 N -0.4491(3) 0.7437(2) 0.2235(2) 0.0430(8) Uani 1 1 d . . .
C11 C -0.0016(4) 0.3329(3) 0.2894(2) 0.0471(11) Uani 1 1 d . . .
C12 C 0.0760(5) 0.3615(4) 0.3857(3) 0.0576(12) Uani 1 1 d . . .
C12A C 0.2174(5) 0.4164(5) 0.4084(3) 0.0784(15) Uani 1 1 d . . .
H12A H 0.2355 0.4461 0.3528 0.108(18) Uiso 1 1 calc R . .
H12B H 0.2734 0.3563 0.4210 0.21(4) Uiso 1 1 calc R . .
H12C H 0.2330 0.4817 0.4656 0.14(2) Uiso 1 1 calc R . .
C13 C 0.0226(7) 0.3370(5) 0.4629(3) 0.0870(18) Uani 1 1 d . . .
H13A H 0.0734 0.3558 0.5268 0.107(17) Uiso 1 1 calc R . .
C14 C -0.1037(7) 0.2856(5) 0.4464(4) 0.097(2) Uani 1 1 d . . .
H14A H -0.1378 0.2694 0.4991 0.120(19) Uiso 1 1 calc R . .
C15 C -0.1806(6) 0.2577(4) 0.3531(4) 0.0789(15) Uani 1 1 d . . .
H15A H -0.2668 0.2236 0.3431 0.092(18) Uiso 1 1 calc R . .
C16 C -0.1309(5) 0.2798(4) 0.2728(3) 0.0576(12) Uani 1 1 d . . .
C16A C -0.2169(5) 0.2436(5) 0.1697(3) 0.0762(15) Uani 1 1 d . . .
H16A H -0.3044 0.2178 0.1739 0.12(2) Uiso 1 1 calc R . .
H16B H -0.1834 0.1788 0.1308 0.18(3) Uiso 1 1 calc R . .
H16C H -0.2172 0.3113 0.1390 0.14(2) Uiso 1 1 calc R . .
C111 C 0.0422(6) 0.6118(4) 0.2726(3) 0.0667(14) Uani 1 1 d . . .
H11A H 0.0349 0.6844 0.2487 0.091(15) Uiso 1 1 calc R . .
H11B H 0.1238 0.6198 0.3191 0.108(19) Uiso 1 1 calc R . .
H11C H -0.0288 0.5980 0.3044 0.13(2) Uiso 1 1 calc R . .
C121 C 0.0804(7) 0.2078(6) 0.0125(3) 0.0948(19) Uani 1 1 d . . .
H12D H 0.1123 0.2770 -0.0088 0.16(3) Uiso 1 1 calc R . .
H12E H -0.0133 0.1947 -0.0066 0.11(2) Uiso 1 1 calc R . .
H12F H 0.1160 0.1383 -0.0177 0.13(2) Uiso 1 1 calc R . .
C122 C 0.3121(5) 0.2665(5) 0.1834(4) 0.0876(17) Uani 1 1 d . . .
H12G H 0.3416 0.2705 0.2528 0.13(2) Uiso 1 1 calc R . .
H12H H 0.3385 0.3422 0.1690 0.19(3) Uiso 1 1 calc R . .
H12I H 0.3499 0.2037 0.1460 0.14(2) Uiso 1 1 calc R . .
C123 C 0.0860(8) 0.0971(4) 0.1929(5) 0.102(2) Uani 1 1 d . . .
H12J H 0.1031 0.1155 0.2638 0.15(3) Uiso 1 1 calc R . .
H12K H 0.1368 0.0351 0.1701 0.14(2) Uiso 1 1 calc R . .
H12L H -0.0052 0.0698 0.1670 0.09(2) Uiso 1 1 calc R . .
C21 C -0.3798(5) 0.7994(3) 0.3237(3) 0.0584(13) Uani 1 1 d . A .
C22 C -0.4444(8) 0.8028(4) 0.4009(3) 0.0913(19) Uani 1 1 d D . .
C22A C -0.5840(9) 0.7483(7) 0.3852(5) 0.127(3) Uani 1 1 d . A .
H22A H -0.6041 0.6835 0.3275 0.17(3) Uiso 1 1 calc R . .
H22B H -0.6411 0.8086 0.3763 0.20(4) Uiso 1 1 calc R . .
H22C H -0.5959 0.7179 0.4419 0.26(5) Uiso 1 1 calc R . .
C23 C -0.362(3) 0.870(3) 0.4899(12) 0.102(9) Uani 0.50(5) 1 d PD A 1
H23A H -0.3993 0.8923 0.5446 0.122 Uiso 0.50(5) 1 calc PR A 1
C24 C -0.227(3) 0.906(3) 0.5014(19) 0.127(13) Uani 0.50(5) 1 d PD A 1
H24A H -0.1794 0.9309 0.5661 0.152 Uiso 0.50(5) 1 calc PR A 1
C25 C -0.156(3) 0.909(3) 0.4264(13) 0.099(9) Uani 0.50(5) 1 d PD A 1
H25A H -0.0696 0.9406 0.4329 0.119 Uiso 0.50(5) 1 calc PR A 1
C23A C -0.403(4) 0.848(4) 0.5043(8) 0.143(11) Uani 0.50(5) 1 d PD A 2
H23B H -0.4489 0.8361 0.5522 0.172 Uiso 0.50(5) 1 calc PR A 2
C24A C -0.278(4) 0.915(3) 0.5212(19) 0.161(19) Uani 0.50(5) 1 d PD A 2
H24B H -0.2385 0.9597 0.5839 0.193 Uiso 0.50(5) 1 calc PR A 2
C25A C -0.216(4) 0.911(4) 0.4406(10) 0.107(12) Uani 0.50(5) 1 d PD A 2
H25B H -0.1348 0.9571 0.4585 0.129 Uiso 0.50(5) 1 calc PR A 2
C26 C -0.2487(7) 0.8532(4) 0.3389(5) 0.090(2) Uani 1 1 d D . .
C26A C -0.1810(7) 0.8550(7) 0.2535(7) 0.120(2) Uani 1 1 d . A .
H26A H -0.1961 0.7765 0.2102 0.23(4) Uiso 1 1 calc R . .
H26B H -0.0887 0.8772 0.2786 0.26(5) Uiso 1 1 calc R . .
H26C H -0.2152 0.9126 0.2176 0.33(7) Uiso 1 1 calc R . .
C211 C -0.3904(5) 0.5175(4) 0.2778(3) 0.0695(14) Uani 1 1 d . . .
H21A H -0.3945 0.4327 0.2511 0.084(14) Uiso 1 1 calc R . .
H21B H -0.4479 0.5307 0.3232 0.12(2) Uiso 1 1 calc R . .
H21C H -0.3024 0.5491 0.3119 0.094(17) Uiso 1 1 calc R . .
C221 C -0.4771(9) 0.8212(8) 0.0344(4) 0.122(2) Uani 1 1 d . . .
H22D H -0.4974 0.7385 -0.0006 0.20(4) Uiso 1 1 calc R . .
H22E H -0.3847 0.8447 0.0456 0.21(5) Uiso 1 1 calc R . .
H22F H -0.5230 0.8710 -0.0042 0.16(3) Uiso 1 1 calc R . .
C222 C -0.7086(5) 0.8058(6) 0.1271(6) 0.104(2) Uani 1 1 d . . .
H22G H -0.7386 0.8095 0.1876 0.14(3) Uiso 1 1 calc R . .
H22H H -0.7338 0.7265 0.0856 0.21(4) Uiso 1 1 calc R . .
H22I H -0.7469 0.8637 0.0935 0.106(17) Uiso 1 1 calc R . .
C223 C -0.4871(7) 0.9962(4) 0.2278(5) 0.103(2) Uani 1 1 d . . .
H22J H -0.5161 1.0029 0.2890 0.18(4) Uiso 1 1 calc R . .
H22K H -0.5296 1.0491 0.1908 0.103(17) Uiso 1 1 calc R . .
H22L H -0.3941 1.0179 0.2415 0.11(2) Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
O11 Si11 O12 104.65(16) . . ?
O11 Si11 N1 105.99(16) . . ?
O12 Si11 N1 114.04(15) . . ?
O11 Si11 C111 112.3(2) . . ?
O12 Si11 C111 107.8(2) . . ?
N1 Si11 C111 111.89(17) . . ?
N1 Si12 C123 108.4(2) . . ?
N1 Si12 C122 112.3(2) . . ?
C123 Si12 C122 107.2(3) . . ?
N1 Si12 C121 110.1(2) . . ?
C123 Si12 C121 110.9(3) . . ?
C122 Si12 C121 107.9(3) . . ?
O21 Si21 O22 102.24(17) . . ?
O21 Si21 N2 108.81(16) . . ?
O22 Si21 N2 114.09(16) . . ?
O21 Si21 C211 114.0(2) . . ?
O22 Si21 C211 107.4(2) . . ?
N2 Si21 C211 110.21(18) . . ?
N2 Si22 C223 109.1(2) . . ?
N2 Si22 C222 112.9(2) . . ?
C223 Si22 C222 107.2(3) . . ?
N2 Si22 C221 109.3(2) . . ?
C223 Si22 C221 111.6(4) . . ?
C222 Si22 C221 106.8(4) . . ?
C11 N1 Si11 118.3(2) . . ?
C11 N1 Si12 116.9(2) . . ?
Si11 N1 Si12 124.79(16) . . ?
C21 N2 Si21 119.4(2) . . ?
C21 N2 Si22 116.2(2) . . ?
Si21 N2 Si22 124.27(16) . . ?
C16 C11 C12 119.8(4) . . ?
C16 C11 N1 119.9(3) . . ?
C12 C11 N1 120.2(4) . . ?
C13 C12 C11 119.2(5) . . ?
C13 C12 C12A 118.4(4) . . ?
C11 C12 C12A 122.4(4) . . ?
C14 C13 C12 120.8(5) . . ?
C13 C14 C15 120.6(5) . . ?
C14 C15 C16 120.7(5) . . ?
C15 C16 C11 118.9(4) . . ?
C15 C16 C16A 119.4(5) . . ?
C11 C16 C16A 121.6(4) . . ?
C22 C21 C26 122.0(5) . . ?
C22 C21 N2 119.4(5) . . ?
C26 C21 N2 118.6(4) . . ?
C21 C22 C23 109.5(14) . . ?
C21 C22 C23A 132.1(19) . . ?
C23 C22 C23A 23.2(18) . . ?
C21 C22 C22A 122.4(5) . . ?
C23 C22 C22A 128.0(15) . . ?
C23A C22 C22A 105.5(19) . . ?
C24 C23 C22 125(2) . . ?
C25 C24 C23 128(2) . . ?
C24 C25 C26 103(2) . . ?
C22 C23A C24A 107(2) . . ?
C25A C24A C23A 118(3) . . ?
C24A C25A C26 135(3) . . ?
C25A C26 C25 28.5(17) . . ?
C25A C26 C21 104(2) . . ?
C25 C26 C21 131.5(15) . . ?
C25A C26 C26A 133(2) . . ?
C25 C26 C26A 106.7(15) . . ?
C21 C26 C26A 121.8(5) . . ?
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
Si11 O11 1.632(3) . ?
Si11 O12 1.643(3) . ?
Si11 N1 1.717(3) . ?
Si11 C111 1.840(4) . ?
Si12 N1 1.754(3) . ?
Si12 C123 1.852(5) . ?
Si12 C122 1.856(5) . ?
Si12 C121 1.863(5) . ?
Si21 O21 1.630(3) . ?
Si21 O22 1.642(3) . ?
Si21 N2 1.717(3) . ?
Si21 C211 1.841(4) . ?
Si22 N2 1.756(3) . ?
Si22 C223 1.843(5) . ?
Si22 C222 1.853(6) . ?
Si22 C221 1.862(6) . ?
N1 C11 1.455(5) . ?
N2 C21 1.451(4) . ?
C11 C16 1.399(6) . ?
C11 C12 1.405(5) . ?
C12 C13 1.385(6) . ?
C12 C12A 1.514(6) . ?
C13 C14 1.364(7) . ?
C14 C15 1.369(7) . ?
C15 C16 1.395(6) . ?
C16 C16A 1.517(6) . ?
C21 C22 1.385(7) . ?
C21 C26 1.420(7) . ?
C22 C23 1.418(7) . ?
C22 C23A 1.416(7) . ?
C22 C22A 1.505(8) . ?
C23 C24 1.412(7) . ?
C24 C25 1.411(8) . ?
C25 C26 1.416(7) . ?
C23A C24A 1.411(7) . ?
C24A C25A 1.412(7) . ?
C25A C26 1.417(7) . ?
C26 C26A 1.517(8) . ?
