#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:52:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180238 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/24/7112493.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_7112493
loop_
_publ_author_name
'Yan Li'
'Hongping Zhu'
'Diego M. Andrada'
'Gernot Frenking'
'Herbert W. Roesky'
_publ_section_title
;
 Aminosilanetrithiol RSi(SH)3: an experimental and quantum-chemical study
;
_journal_name_full               Chem.Commun.
_journal_page_first              4628
_journal_paper_doi               10.1039/C4CC00912f
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C15 H29 N S3 Si2'
_chemical_formula_weight         375.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1294(9)
_cell_length_b                   12.0775(7)
_cell_length_c                   14.2602(8)
_cell_measurement_reflns_used    2439
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.3137
_cell_measurement_theta_min      2.7701
_cell_volume                     2089.0(2)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_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      173(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhanced (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7290
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.9210
_exptl_absorpt_correction_T_min  0.8732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2077
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0434P)²+1.5806P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1057
_reflns_number_gt                1650
_reflns_number_total             2077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc00912f2.cif
_cod_data_source_block           compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      Cmc2(1)
_cod_database_code               7112493
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, 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
N1 N 1.0000 0.3480(2) 0.9646(7) 0.0323(7) Uani 1 2 d SD . .
C1 C 1.0000 0.2273(3) 0.9634(9) 0.0265(7) Uani 1 2 d S A .
C2 C 1.0000 0.1708(7) 1.0477(6) 0.031(2) Uani 1 2 d S . .
C3 C 1.0000 0.0574(10) 1.0475(7) 0.045(2) Uani 1 2 d S A .
H3A H 1.0000 0.0186 1.1055 0.054 Uiso 1 2 calc SR . .
C4 C 1.0000 -0.0021(3) 0.9637(10) 0.0443(11) Uani 1 2 d S . .
H4A H 1.0000 -0.0808 0.9646 0.053 Uiso 1 2 calc SR A .
C5 C 1.0000 0.0531(7) 0.8811(7) 0.036(2) Uani 1 2 d S A .
H5A H 1.0000 0.0120 0.8243 0.043 Uiso 1 2 calc SR . .
C6 C 1.0000 0.1696(8) 0.8767(6) 0.0287(19) Uani 1 2 d S . .
C7 C 1.0000 0.2283(9) 1.1459(7) 0.038(2) Uani 1 2 d S . .
H7A H 1.0000 0.3102 1.1357 0.045 Uiso 1 2 calc SR . .
C8 C 1.1031(7) 0.1986(7) 1.2017(5) 0.058(2) Uani 1 1 d . . .
H8A H 1.1008 0.2354 1.2629 0.087 Uiso 1 1 calc R A .
H8B H 1.1687 0.2230 1.1672 0.087 Uiso 1 1 calc R . .
H8C H 1.1062 0.1182 1.2107 0.087 Uiso 1 1 calc R . .
C9 C 1.0000 0.2263(9) 0.7859(7) 0.040(2) Uani 1 2 d S . .
H9A H 1.0000 0.3078 0.7983 0.048 Uiso 1 2 calc SR . .
C10 C 0.8978(8) 0.1994(7) 0.7284(5) 0.057(2) Uani 1 1 d . . .
H10A H 0.9002 0.2404 0.6691 0.085 Uiso 1 1 calc R A .
H10B H 0.8318 0.2207 0.7636 0.085 Uiso 1 1 calc R . .
H10C H 0.8957 0.1198 0.7154 0.085 Uiso 1 1 calc R . .
Si2 Si 0.8671(6) 0.4118(6) 0.9690(7) 0.0506(14) Uani 0.50 1 d PDU A 2
C11 C 0.8841(13) 0.5361(10) 1.0552(8) 0.063(2) Uani 0.50 1 d PDU A 2
H11A H 0.9170 0.5100 1.1139 0.094 Uiso 0.50 1 calc PR A 2
H11B H 0.8117 0.5687 1.0682 0.094 Uiso 0.50 1 calc PR A 2
H11C H 0.9321 0.5921 1.0268 0.094 Uiso 0.50 1 calc PR A 2
C12 C 0.8320(15) 0.4869(12) 0.8585(10) 0.064(2) Uani 0.50 1 d PDU A 2
H12A H 0.8289 0.4341 0.8063 0.097 Uiso 0.50 1 calc PR A 2
H12B H 0.8885 0.5428 0.8456 0.097 Uiso 0.50 1 calc PR A 2
H12C H 0.7601 0.5230 0.8655 0.097 Uiso 0.50 1 calc PR A 2
C13 C 0.7548(12) 0.3151(10) 0.9887(12) 0.060(2) Uani 0.50 1 d PDU A 2
H13A H 0.7688 0.2467 0.9537 0.090 Uiso 0.50 1 calc PR A 2
H13B H 0.6855 0.3482 0.9673 0.090 Uiso 0.50 1 calc PR A 2
H13C H 0.7496 0.2982 1.0558 0.090 Uiso 0.50 1 calc PR A 2
Si1 Si 0.8771(6) 0.4141(6) 0.9618(5) 0.0444(12) Uani 0.50 1 d PDU A 1
S1 S 0.8473(5) 0.5074(5) 1.0844(3) 0.0788(12) Uani 0.50 1 d PDU A 1
H1 H 0.740(3) 0.532(7) 1.077(5) 0.05(2) Uiso 0.50 1 d PD B 1
S2 S 0.8637(5) 0.5237(4) 0.8479(3) 0.0830(14) Uani 0.50 1 d PDU A 1
H2 H 0.851(7) 0.444(4) 0.786(4) 0.04(2) Uiso 0.50 1 d PD C 1
S3 S 0.7546(3) 0.2912(3) 0.9600(5) 0.0609(8) Uani 0.50 1 d PDU A 1
H3 H 0.769(6) 0.225(6) 1.034(4) 0.05(2) Uiso 0.50 1 d PD D 1
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
C1 N1 Si1 118.2(3) . 4_755
C1 N1 Si1 118.2(3) . .
Si1 N1 Si1 123.6(6) 4_755 .
C1 N1 Si2 115.6(3) . 4_755
Si1 N1 Si2 4.2(6) 4_755 4_755
Si1 N1 Si2 126.29(16) . 4_755
C1 N1 Si2 115.6(3) . .
Si1 N1 Si2 126.29(16) 4_755 .
Si1 N1 Si2 4.2(6) . .
Si2 N1 Si2 128.7(5) 4_755 .
C2 C1 C6 121.0(3) . .
C2 C1 N1 118.9(9) . .
C6 C1 N1 120.1(8) . .
C3 C2 C1 119.5(8) . .
C3 C2 C7 116.5(8) . .
C1 C2 C7 124.0(7) . .
C2 C3 C4 121.2(8) . .
C2 C3 H3A 119.4 . .
C4 C3 H3A 119.4 . .
C5 C4 C3 119.4(4) . .
C5 C4 H4A 120.3 . .
C3 C4 H4A 120.3 . .
C4 C5 C6 122.1(8) . .
C4 C5 H5A 119.0 . .
C6 C5 H5A 119.0 . .
C5 C6 C1 116.8(9) . .
C5 C6 C9 120.4(8) . .
C1 C6 C9 122.7(8) . .
C8 C7 C8 110.2(10) . 4_755
C8 C7 C2 111.2(6) . .
C8 C7 C2 111.2(6) 4_755 .
C8 C7 H7A 108.0 . .
C8 C7 H7A 108.0 4_755 .
C2 C7 H7A 108.0 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C6 C9 C10 112.1(6) . .
C6 C9 C10 112.1(6) . 4_755
C10 C9 C10 109.1(9) . 4_755
C6 C9 H9A 107.8 . .
C10 C9 H9A 107.8 . .
C10 C9 H9A 107.8 4_755 .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N1 Si2 C13 113.9(7) . .
N1 Si2 C12 112.7(8) . .
C13 Si2 C12 105.8(9) . .
N1 Si2 C11 105.0(6) . .
C13 Si2 C11 118.4(7) . .
C12 Si2 C11 100.5(8) . .
Si2 C11 H11A 109.5 . .
Si2 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
Si2 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
Si2 C12 H12A 109.5 . .
Si2 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
Si2 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
Si2 C12 H2 119(4) . .
H12A C12 H2 19.3 . .
H12B C12 H2 90.2 . .
H12C C12 H2 117.2 . .
Si2 C13 H13A 109.5 . .
Si2 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
Si2 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
Si2 C13 H3 122(4) . .
H13A C13 H3 60.9 . .
H13B C13 H3 128.5 . .
H13C C13 H3 48.7 . .
N1 Si1 S3 106.8(4) . .
N1 Si1 S2 112.5(5) . .
S3 Si1 S2 112.4(4) . .
N1 Si1 S1 112.6(5) . .
S3 Si1 S1 105.5(4) . .
S2 Si1 S1 106.9(4) . .
Si1 S1 H1 103(3) . .
Si1 S2 H2 94(3) . .
Si1 S3 H3 109(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C1 1.457(4) .
N1 Si1 1.692(7) 4_755
N1 Si1 1.692(7) .
N1 Si2 1.788(8) 4_755
N1 Si2 1.788(8) .
C1 C2 1.384(15) .
C1 C6 1.419(14) .
C2 C3 1.369(15) .
C2 C7 1.563(13) .
C3 C4 1.396(16) .
C3 H3A 0.9500 .
C4 C5 1.354(15) .
C4 H4A 0.9500 .
C5 C6 1.409(13) .
C5 H5A 0.9500 .
C6 C9 1.464(14) .
C7 C8 1.525(10) .
C7 C8 1.525(10) 4_755
C7 H7A 1.0000 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.521(11) .
C9 C10 1.521(11) 4_755
C9 H9A 1.0000 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
Si2 C13 1.816(10) .
Si2 C12 1.867(10) .
Si2 C11 1.952(10) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C12 H2 1.18(5) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C13 H3 1.28(5) .
Si1 S3 2.101(7) .
Si1 S2 2.101(8) .
Si1 S1 2.110(7) .
S1 H1 1.34(3) .
S2 H2 1.31(3) .
S3 H3 1.34(3) .
