#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:07:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179880 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/76/7017657.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_7017657
loop_
_publ_author_name
'Kobelt, Claudia'
'Burschka, Christian'
'Bertermann, Rüdiger'
'Fonseca Guerra, C.'
'Bickelhaupt, F. Matthias'
'Tacke, Reinhold'
_publ_section_title
;
 Synthesis and structural characterisation of neutral pentacoordinate
 silicon(iv) complexes with a tridentate dianionic N,N,S chelate ligand.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2148
_journal_page_last               2162
_journal_paper_doi               10.1039/c1dt11306b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C13 H13 Cl N2 S Si'
_chemical_formula_sum            'C13 H13 Cl N2 S Si'
_chemical_formula_weight         292.85
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.328(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1864(15)
_cell_length_b                   9.7269(19)
_cell_length_c                   18.971(4)
_cell_measurement_reflns_used    9761
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.23
_cell_measurement_theta_min      2.35
_cell_volume                     1318.0(5)
_computing_cell_refinement       Bruker-SAINT
_computing_data_collection       Bruker-SAINT
_computing_data_reduction        Bruker-SAINT
_computing_molecular_graphics    Ortep/Povray
_computing_publication_material  Bruker-SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  Bruker-Kappa_Apex2_CCD
_diffrn_measurement_method       omega_and_phi_scans
_diffrn_radiation_monochromator  Montel_multi_layer_optics
_diffrn_radiation_source         rotating_anode
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35821
_diffrn_reflns_theta_full        32.36
_diffrn_reflns_theta_max         32.36
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  .7463
_exptl_absorpt_correction_T_min  .6666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flat_needle
_exptl_crystal_F_000             608
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .17
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         4669
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0270P)²+0.9168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                4218
_reflns_number_total             4669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11306b.txt
_cod_data_source_block           kob14lu_7
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7017657
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
S S 0.26442(5) 1.28277(3) 0.215680(17) 0.01911(7) Uani 1 1 d . . .
Si Si 0.25522(5) 1.07677(3) 0.161225(18) 0.01558(8) Uani 0.50 1 d PD A 1
Cl Cl 0.49453(10) 1.12676(10) 0.10980(5) 0.02061(12) Uani 0.7113(13) 1 d PD A 1
C1 C 0.0433(5) 1.1066(7) 0.0967(2) 0.02159(11) Uani 0.7113(13) 1 d PD A 1
H1D H 0.0376 1.0368 0.0592 0.032 Uiso 0.7113(13) 1 calc PR A 1
H1E H 0.0504 1.1981 0.0756 0.032 Uiso 0.7113(13) 1 calc PR A 1
H1F H -0.0693 1.1004 0.1213 0.032 Uiso 0.7113(13) 1 calc PR A 1
SiB Si 0.25522(5) 1.07677(3) 0.161225(18) 0.01558(8) Uani 0.50 1 d PD A 2
ClB Cl 0.0174(2) 1.1124(4) 0.08977(11) 0.02159(11) Uani 0.2887(13) 1 d PD A 2
C1B C 0.4641(13) 1.1210(13) 0.1147(6) 0.02061(12) Uani 0.2887(13) 1 d PD A 2
H1A H 0.5785 1.1070 0.1471 0.031 Uiso 0.2887(13) 1 calc PR A 2
H1B H 0.4561 1.2173 0.0996 0.031 Uiso 0.2887(13) 1 calc PR A 2
H1C H 0.4669 1.0616 0.0731 0.031 Uiso 0.2887(13) 1 calc PR A 2
N2 N 0.23653(15) 0.99948(11) 0.24340(5) 0.01671(19) Uani 1 1 d . . .
N1 N 0.27902(15) 0.88344(11) 0.13076(6) 0.0176(2) Uani 1 1 d . . .
C7 C 0.21797(17) 1.07529(13) 0.30483(6) 0.0166(2) Uani 1 1 d . A .
C2 C 0.22969(17) 1.21887(13) 0.29939(7) 0.0173(2) Uani 1 1 d . A .
C8 C 0.23589(18) 0.85131(12) 0.25136(6) 0.0173(2) Uani 1 1 d . A .
H8A H 0.1141 0.8202 0.2654 0.021 Uiso 1 1 calc R . .
H8B H 0.3360 0.8225 0.2885 0.021 Uiso 1 1 calc R . .
C3 C 0.21526(19) 1.30161(14) 0.35801(7) 0.0221(2) Uani 1 1 d . . .
H3 H 0.2243 1.3987 0.3539 0.026 Uiso 1 1 calc R A .
C9 C 0.26807(17) 0.79063(13) 0.18203(7) 0.0172(2) Uani 1 1 d . A .
C10 C 0.28778(19) 0.65072(13) 0.17035(7) 0.0215(2) Uani 1 1 d . . .
H10 H 0.2800 0.5864 0.2076 0.026 Uiso 1 1 calc R A .
C6 C 0.18966(19) 1.01717(15) 0.37014(7) 0.0212(2) Uani 1 1 d . . .
H6 H 0.1812 0.9202 0.3748 0.025 Uiso 1 1 calc R A .
C11 C 0.3190(2) 0.60716(15) 0.10330(8) 0.0254(3) Uani 1 1 d . A .
H11 H 0.3346 0.5121 0.0940 0.030 Uiso 1 1 calc R . .
C12 C 0.3273(2) 0.70354(15) 0.04971(8) 0.0257(3) Uani 1 1 d . . .
H12 H 0.3473 0.6751 0.0032 0.031 Uiso 1 1 calc R A .
C5 C 0.1739(2) 1.10183(16) 0.42857(7) 0.0247(3) Uani 1 1 d . A .
H5 H 0.1535 1.0619 0.4728 0.030 Uiso 1 1 calc R . .
C4 C 0.1876(2) 1.24282(16) 0.42296(7) 0.0256(3) Uani 1 1 d . A .
H4 H 0.1781 1.2995 0.4632 0.031 Uiso 1 1 calc R . .
C13 C 0.3065(2) 0.84037(14) 0.06479(7) 0.0224(2) Uani 1 1 d . A .
H13 H 0.3114 0.9063 0.0281 0.027 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'
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
C2 S Si 95.76(5)
N2 Si C1 120.91(16)
N2 Si N1 82.50(5)
C1 Si N1 92.7(2)
N2 Si Cl 130.77(5)
C1 Si Cl 107.81(13)
N1 Si Cl 89.03(4)
N2 Si S 88.56(4)
C1 Si S 98.2(2)
N1 Si S 168.44(4)
Cl Si S 91.30(3)
C7 N2 C8 115.85(10)
C7 N2 Si 122.69(9)
C8 N2 Si 121.46(8)
C9 N1 C13 119.34(11)
C9 N1 Si 114.54(9)
C13 N1 Si 126.11(9)
C6 C7 N2 124.24(12)
C6 C7 C2 118.93(12)
N2 C7 C2 116.84(11)
C3 C2 C7 120.55(12)
C3 C2 S 123.59(10)
C7 C2 S 115.86(9)
N2 C8 C9 107.50(10)
C2 C3 C4 120.15(13)
N1 C9 C10 122.07(12)
N1 C9 C8 113.85(11)
C10 C9 C8 124.07(11)
C11 C10 C9 118.49(13)
C5 C6 C7 119.88(13)
C10 C11 C12 119.42(13)
C13 C12 C11 119.15(13)
C4 C5 C6 120.83(13)
C5 C4 C3 119.65(13)
N1 C13 C12 121.51(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S C2 1.7486(13)
S Si 2.2520(6)
Si N2 1.7492(11)
Si C1 1.869(4)
Si N1 1.9803(12)
Si Cl 2.1250(6)
N2 C7 1.3980(16)
N2 C8 1.4492(16)
N1 C9 1.3357(16)
N1 C13 1.3546(16)
C7 C6 1.3970(17)
C7 C2 1.4036(17)
C2 C3 1.3860(18)
C8 C9 1.4828(17)
C3 C4 1.392(2)
C9 C10 1.3886(18)
C10 C11 1.382(2)
C6 C5 1.3955(19)
C11 C12 1.389(2)
C12 C13 1.373(2)
C5 C4 1.380(2)
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
C2 S Si N2 -3.95(6)
C2 S Si C1 117.09(15)
C2 S Si N1 -43.21(19)
C2 S Si Cl -134.70(5)
C1 Si N2 C7 -93.3(3)
N1 Si N2 C7 178.10(10)
Cl Si N2 C7 95.93(11)
S Si N2 C7 5.45(10)
C1 Si N2 C8 85.5(3)
N1 Si N2 C8 -3.09(10)
Cl Si N2 C8 -85.27(11)
S Si N2 C8 -175.74(10)
N2 Si N1 C9 0.88(9)
C1 Si N1 C9 -119.95(17)
Cl Si N1 C9 132.26(9)
S Si N1 C9 40.5(2)
N2 Si N1 C13 -178.37(12)
C1 Si N1 C13 60.79(18)
Cl Si N1 C13 -47.00(11)
S Si N1 C13 -138.72(16)
C8 N2 C7 C6 -3.53(18)
Si N2 C7 C6 175.34(10)
C8 N2 C7 C2 176.22(11)
Si N2 C7 C2 -4.91(16)
C6 C7 C2 C3 0.63(19)
N2 C7 C2 C3 -179.14(12)
C6 C7 C2 S -179.79(10)
N2 C7 C2 S 0.45(15)
Si S C2 C3 -177.76(11)
Si S C2 C7 2.67(10)
C7 N2 C8 C9 -176.72(10)
Si N2 C8 C9 4.39(14)
C7 C2 C3 C4 -0.5(2)
S C2 C3 C4 179.99(11)
C13 N1 C9 C10 1.35(19)
Si N1 C9 C10 -177.96(10)
C13 N1 C9 C8 -179.39(11)
Si N1 C9 C8 1.30(14)
N2 C8 C9 N1 -3.29(15)
N2 C8 C9 C10 175.95(12)
N1 C9 C10 C11 -0.2(2)
C8 C9 C10 C11 -179.43(12)
N2 C7 C6 C5 179.64(12)
C2 C7 C6 C5 -0.11(19)
C9 C10 C11 C12 -0.8(2)
C10 C11 C12 C13 0.7(2)
C7 C6 C5 C4 -0.6(2)
C6 C5 C4 C3 0.8(2)
C2 C3 C4 C5 -0.2(2)
C9 N1 C13 C12 -1.4(2)
Si N1 C13 C12 177.80(11)
C11 C12 C13 N1 0.4(2)
