#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:01:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179463 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/60/4336093.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_4336093
loop_
_publ_author_name
'Johannes A. Baus'
'Christian Burschka'
'Rüdiger Bertermann'
'Célia Fonseca Guerra'
'F. Matthias Bickelhaupt'
'Reinhold Tacke'
_publ_contact_author_address
;Institut fuer Anorganische Chemie
 Julius-Maximilians-Universitaet Wuerzburg
 Am Hubland
 D-97074 Wuerzburg
 Germany,
 Department of Theoretical Chemistry,
 Amsterdam Center for Multiscale Modeling (ACMM), VU University Amsterdam
 De Boelelaan 1083
 NL-1081 HV Amsterdam
 The Netherlands
;
_publ_contact_author_email       r.tacke@uni-wuerzburg.de,f.m.bickelhaupt@vu.nl
_publ_contact_author_fax         '049 931 3184609, 031 20 5987629'
_publ_contact_author_name        'Reinhold Tacke, F. Matthias Bickelhaupt'
_publ_contact_author_phone       '049 931 3185251, 031 20 5987617'
_publ_section_title
;
 Neutral Six-Coordinate and Cationic Five-Coordinate Silicon(IV) Complexes
 with Two Bidentate Monoanionic N,S-Pyridine-2-thiolato(-) Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10664
_journal_page_last               10676
_journal_paper_doi               10.1021/ic401698a
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C10 H8 Cl2 N2 S2 Si'
_chemical_formula_sum            'C10 H8 Cl2 N2 S2 Si'
_chemical_formula_weight         319.29
_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                82.61(3)
_cell_angle_beta                 86.81(3)
_cell_angle_gamma                67.85(3)
_cell_formula_units_Z            2
_cell_length_a                   7.1234(14)
_cell_length_b                   8.0698(16)
_cell_length_c                   12.208(2)
_cell_measurement_reflns_used    4188
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.75
_cell_volume                     644.6(3)
_computing_cell_refinement       STOE-IPDS
_computing_data_collection       STOE-IPDS
_computing_data_reduction        STOE-IPDS
_computing_molecular_graphics    ORTEP/POV-Ray
_computing_publication_material  Bruker-SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  image-plate_STOE-IPDS
_diffrn_measurement_method       'omega scan'
_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  0.0918
_diffrn_reflns_av_sigmaI/netI    0.1128
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8469
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       plate
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.838
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0424P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                1600
_reflns_number_total             2852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401698a_si_002_2.cif
_cod_data_source_block           bau02b
_cod_original_cell_volume        644.5(2)
_cod_database_code               4336093
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
C1 C 0.6795(6) 0.5941(5) 0.2988(3) 0.0250(8) Uani 1 1 d .
C2 C 0.5153(6) 0.7372(5) 0.3337(3) 0.0291(9) Uani 1 1 d .
H2 H 0.5171 0.8552 0.3259 0.035 Uiso 1 1 calc R
C3 C 0.3498(6) 0.7043(5) 0.3799(3) 0.0325(9) Uani 1 1 d .
H3 H 0.2368 0.8003 0.4046 0.039 Uiso 1 1 calc R
C4 C 0.3471(6) 0.5301(5) 0.3905(3) 0.0298(9) Uani 1 1 d .
H4 H 0.2318 0.5078 0.4207 0.036 Uiso 1 1 calc R
C5 C 0.5133(6) 0.3926(5) 0.3568(3) 0.0260(9) Uani 1 1 d .
H5 H 0.5143 0.2736 0.3646 0.031 Uiso 1 1 calc R
C6 C 0.8111(6) 0.1314(5) 0.1308(3) 0.0254(8) Uani 1 1 d .
C7 C 0.7400(6) 0.0725(5) 0.0447(3) 0.0291(9) Uani 1 1 d .
H7 H 0.7251 -0.0406 0.0537 0.035 Uiso 1 1 calc R
C8 C 0.6919(6) 0.1846(5) -0.0539(3) 0.0318(9) Uani 1 1 d .
H8 H 0.6444 0.1476 -0.1140 0.038 Uiso 1 1 calc R
C9 C 0.7124(6) 0.3507(5) -0.0661(3) 0.0311(9) Uani 1 1 d .
H9 H 0.6783 0.4272 -0.1339 0.037 Uiso 1 1 calc R
C10 C 0.7825(6) 0.4034(5) 0.0210(3) 0.0274(9) Uani 1 1 d .
H10 H 0.7979 0.5162 0.0133 0.033 Uiso 1 1 calc R
Cl1 Cl 1.06807(15) 0.22300(12) 0.42416(8) 0.0301(2) Uani 1 1 d .
Cl2 Cl 1.24801(15) 0.20699(12) 0.18002(8) 0.0292(2) Uani 1 1 d .
N1 N 0.6770(5) 0.4251(4) 0.3122(2) 0.0240(7) Uani 1 1 d .
N2 N 0.8292(5) 0.2949(4) 0.1173(2) 0.0235(7) Uani 1 1 d .
S1 S 0.90702(16) 0.58436(12) 0.23614(8) 0.0280(2) Uani 1 1 d .
S2 S 0.89504(16) 0.02880(12) 0.26173(8) 0.0290(2) Uani 1 1 d .
Si Si 0.94774(16) 0.28982(12) 0.25836(8) 0.0232(2) Uani 1 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 0.0033 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'
Cl Cl 0.1484 0.1585 '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
N1 C1 C2 120.2(4)
N1 C1 S1 108.1(3)
C2 C1 S1 131.7(3)
C3 C2 C1 118.7(3)
C2 C3 C4 120.5(4)
C5 C4 C3 118.9(4)
N1 C5 C4 120.5(3)
N2 C6 C7 120.5(3)
N2 C6 S2 108.0(2)
C7 C6 S2 131.5(3)
C8 C7 C6 117.8(3)
C7 C8 C9 120.8(3)
C10 C9 C8 119.4(4)
N2 C10 C9 120.0(3)
C5 N1 C1 121.2(3)
C5 N1 Si 138.5(2)
C1 N1 Si 100.3(2)
C10 N2 C6 121.5(3)
C10 N2 Si 137.7(2)
C6 N2 Si 100.6(2)
C1 S1 Si 78.71(12)
C6 S2 Si 78.87(12)
N2 Si N1 88.79(13)
N2 Si Cl1 166.01(10)
N1 Si Cl1 91.56(10)
N2 Si Cl2 89.44(10)
N1 Si Cl2 165.21(10)
Cl1 Si Cl2 93.69(6)
N2 Si S1 95.72(10)
N1 Si S1 72.74(10)
Cl1 Si S1 97.73(6)
Cl2 Si S1 92.84(6)
N2 Si S2 72.55(9)
N1 Si S2 94.69(10)
Cl1 Si S2 93.49(6)
Cl2 Si S2 98.77(6)
S1 Si S2 163.29(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.359(4)
C1 C2 1.392(5)
C1 S1 1.732(4)
C2 C3 1.378(6)
C3 C4 1.403(5)
C4 C5 1.370(5)
C5 N1 1.359(5)
C6 N2 1.362(4)
C6 C7 1.398(5)
C6 S2 1.729(4)
C7 C8 1.385(5)
C8 C9 1.390(5)
C9 C10 1.378(5)
C10 N2 1.348(5)
Cl1 Si 2.1648(15)
Cl2 Si 2.1897(16)
N1 Si 1.949(3)
N2 Si 1.949(3)
S1 Si 2.2649(13)
S2 Si 2.2697(13)
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
N1 C1 C2 C3 -1.2(5)
S1 C1 C2 C3 178.7(3)
C1 C2 C3 C4 -0.5(5)
C2 C3 C4 C5 1.5(5)
C3 C4 C5 N1 -1.0(5)
N2 C6 C7 C8 0.9(6)
S2 C6 C7 C8 -177.0(3)
C6 C7 C8 C9 -0.6(6)
C7 C8 C9 C10 0.4(6)
C8 C9 C10 N2 -0.5(6)
C4 C5 N1 C1 -0.7(5)
C4 C5 N1 Si 176.4(3)
C2 C1 N1 C5 1.8(5)
S1 C1 N1 C5 -178.1(2)
C2 C1 N1 Si -176.3(3)
S1 C1 N1 Si 3.8(2)
C9 C10 N2 C6 0.8(6)
C9 C10 N2 Si 174.5(3)
C7 C6 N2 C10 -1.0(5)
S2 C6 N2 C10 177.4(3)
C7 C6 N2 Si -176.7(3)
S2 C6 N2 Si 1.7(3)
N1 C1 S1 Si -3.3(2)
C2 C1 S1 Si 176.8(4)
N2 C6 S2 Si -1.4(2)
C7 C6 S2 Si 176.6(4)
C10 N2 Si N1 88.9(4)
C6 N2 Si N1 -96.6(2)
C10 N2 Si Cl1 -179.5(3)
C6 N2 Si Cl1 -5.0(6)
C10 N2 Si Cl2 -76.4(4)
C6 N2 Si Cl2 98.1(2)
C10 N2 Si S1 16.4(4)
C6 N2 Si S1 -169.1(2)
C10 N2 Si S2 -175.8(4)
C6 N2 Si S2 -1.3(2)
C5 N1 Si N2 83.2(3)
C1 N1 Si N2 -99.3(2)
C5 N1 Si Cl1 -82.8(3)
C1 N1 Si Cl1 94.7(2)
C5 N1 Si Cl2 166.4(3)
C1 N1 Si Cl2 -16.1(5)
C5 N1 Si S1 179.6(4)
C1 N1 Si S1 -2.90(18)
C5 N1 Si S2 10.8(3)
C1 N1 Si S2 -171.7(2)
C1 S1 Si N2 89.23(16)
C1 S1 Si N1 2.29(14)
C1 S1 Si Cl1 -86.94(13)
C1 S1 Si Cl2 178.95(12)
C1 S1 Si S2 44.8(2)
C6 S2 Si N2 1.00(16)
C6 S2 Si N1 88.25(16)
C6 S2 Si Cl1 -179.90(14)
C6 S2 Si Cl2 -85.62(14)
C6 S2 Si S1 47.9(3)
