#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/76/7017651.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_7017651
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         '2(C18 H15 Cl N2 S Si), C7 H8'
_chemical_formula_sum            'C21.5 H19 Cl N2 S Si'
_chemical_formula_weight         400.99
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 120.487(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.132(3)
_cell_length_b                   12.5246(17)
_cell_length_c                   17.107(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.7
_cell_measurement_theta_min      6.65
_cell_volume                     3901.7(10)
_computing_cell_refinement       Stoe-IPDS
_computing_data_collection       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_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      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24326
_diffrn_reflns_theta_full        29.11
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.8423
_exptl_absorpt_correction_T_min  0.7832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       oktahedron
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .5
_exptl_crystal_size_min          .4
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         5193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0366
_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)+(0.0495P)²+2.8691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                4263
_reflns_number_total             5193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11306b.txt
_cod_data_source_block           kob03e_compound_1_x_0.5_C7H8
_cod_original_cell_volume        3901.6(9)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C21.50 H19 Cl N2 S Si'
_cod_database_code               7017651
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
C1 C 0.16011(8) 0.54716(11) 0.10257(9) 0.0230(3) Uani 1 1 d .
C2 C 0.09192(9) 0.56287(14) 0.02393(11) 0.0350(3) Uani 1 1 d .
H2 H 0.0798 0.5231 -0.0291 0.042 Uiso 1 1 calc R
C3 C 0.04143(9) 0.63590(15) 0.02214(12) 0.0408(4) Uani 1 1 d .
H3 H -0.0046 0.6455 -0.0319 0.049 Uiso 1 1 calc R
C4 C 0.05819(10) 0.69458(13) 0.09912(12) 0.0354(3) Uani 1 1 d .
H4 H 0.0234 0.7435 0.0982 0.042 Uiso 1 1 calc R
C5 C 0.12581(9) 0.68149(12) 0.17729(11) 0.0306(3) Uani 1 1 d .
H5 H 0.1378 0.7224 0.2298 0.037 Uiso 1 1 calc R
C6 C 0.17639(8) 0.60838(11) 0.17909(9) 0.0258(3) Uani 1 1 d .
H6 H 0.2226 0.6000 0.2331 0.031 Uiso 1 1 calc R
C7 C 0.30441(8) 0.62119(12) 0.08025(11) 0.0306(3) Uani 1 1 d .
H7 H 0.3179 0.6417 0.1402 0.037 Uiso 1 1 calc R
C8 C 0.32754(9) 0.68269(13) 0.03214(12) 0.0364(4) Uani 1 1 d .
H8 H 0.3575 0.7438 0.0591 0.044 Uiso 1 1 calc R
C9 C 0.30624(10) 0.65363(14) -0.05629(13) 0.0392(4) Uani 1 1 d .
H9 H 0.3216 0.6947 -0.0904 0.047 Uiso 1 1 calc R
C10 C 0.26246(10) 0.56444(13) -0.09442(11) 0.0345(3) Uani 1 1 d .
H10 H 0.2463 0.5446 -0.1553 0.041 Uiso 1 1 calc R
C11 C 0.24249(8) 0.50416(12) -0.04155(9) 0.0256(3) Uani 1 1 d .
C12 C 0.19726(8) 0.40480(12) -0.07262(9) 0.0259(3) Uani 1 1 d .
H12A H 0.1485 0.4203 -0.1261 0.031 Uiso 1 1 calc R
H12B H 0.2218 0.3502 -0.0899 0.031 Uiso 1 1 calc R
C13 C 0.14928(8) 0.27065(11) -0.01291(10) 0.0244(3) Uani 1 1 d .
C14 C 0.11579(9) 0.21349(13) -0.09455(11) 0.0308(3) Uani 1 1 d .
H14 H 0.1187 0.2393 -0.1448 0.037 Uiso 1 1 calc R
C15 C 0.07809(9) 0.11880(13) -0.10242(12) 0.0367(4) Uani 1 1 d .
H15 H 0.0557 0.0806 -0.1581 0.044 Uiso 1 1 calc R
C16 C 0.07292(9) 0.07996(13) -0.03030(13) 0.0372(4) Uani 1 1 d .
H16 H 0.0468 0.0158 -0.0366 0.045 Uiso 1 1 calc R
C17 C 0.10637(9) 0.13568(13) 0.05219(12) 0.0327(3) Uani 1 1 d .
H17 H 0.1033 0.1089 0.1021 0.039 Uiso 1 1 calc R
C18 C 0.14411(8) 0.23019(11) 0.06093(10) 0.0260(3) Uani 1 1 d .
C19 C 0.5000 0.6400(2) 0.2500 0.0613(9) Uani 1 2 d S
H19A H 0.5070 0.6140 0.3079 0.092 Uiso 0.50 1 calc PR
H19B H 0.5400 0.6140 0.2418 0.092 Uiso 0.50 1 calc PR
H19C H 0.4530 0.6140 0.2003 0.092 Uiso 0.50 1 calc PR
C20 C 0.5000 0.7613(2) 0.2500 0.0351(5) Uani 1 2 d S
C21 C 0.54456(10) 0.81827(16) 0.22715(12) 0.0409(4) Uani 1 1 d .
H21 H 0.5757 0.7807 0.2117 0.049 Uiso 1 1 calc R
C22 C 0.54457(11) 0.92885(17) 0.22645(13) 0.0479(5) Uani 1 1 d .
H22 H 0.5751 0.9663 0.2099 0.057 Uiso 1 1 calc R
C23 C 0.5000 0.9850(2) 0.2500 0.0519(7) Uani 1 2 d S
H23 H 0.5000 1.0608 0.2500 0.062 Uiso 1 2 calc SR
Cl Cl 0.325265(19) 0.45497(3) 0.22724(2) 0.02867(9) Uani 1 1 d .
N1 N 0.26306(6) 0.53254(10) 0.04390(8) 0.0240(2) Uani 1 1 d .
N2 N 0.18899(7) 0.36584(10) 0.00197(8) 0.0235(2) Uani 1 1 d .
S S 0.19185(2) 0.30310(3) 0.16237(2) 0.02977(10) Uani 1 1 d .
Si Si 0.22236(2) 0.44008(3) 0.10296(2) 0.02131(9) 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
_geom_angle_site_symmetry_1
C2 C1 C6 117.80(13) .
C2 C1 Si 118.82(11) .
C6 C1 Si 123.26(11) .
C3 C2 C1 121.12(15) .
C4 C3 C2 120.17(16) .
C5 C4 C3 119.67(14) .
C4 C5 C6 120.16(14) .
C5 C6 C1 121.07(14) .
N1 C7 C8 121.58(15) .
C7 C8 C9 118.95(16) .
C10 C9 C8 119.60(15) .
C9 C10 C11 118.68(15) .
N1 C11 C10 121.57(14) .
N1 C11 C12 113.76(12) .
C10 C11 C12 124.66(13) .
N2 C12 C11 107.87(11) .
C14 C13 N2 124.60(13) .
C14 C13 C18 118.56(14) .
N2 C13 C18 116.83(12) .
C15 C14 C13 120.35(15) .
C16 C15 C14 120.84(15) .
C15 C16 C17 119.73(15) .
C18 C17 C16 120.01(15) .
C17 C18 C13 120.51(14) .
C17 C18 S 123.96(12) .
C13 C18 S 115.45(11) .
C21 C20 C21 118.1(2) 2_655
C21 C20 C19 120.96(12) 2_655
C21 C20 C19 120.96(12) .
C22 C21 C20 121.33(18) .
C21 C22 C23 120.04(19) .
C22 C23 C22 119.2(3) 2_655
C11 N1 C7 119.58(13) .
C11 N1 Si 114.35(10) .
C7 N1 Si 125.95(10) .
C13 N2 C12 116.84(11) .
C13 N2 Si 122.01(9) .
C12 N2 Si 121.02(10) .
C18 S Si 95.90(5) .
N2 Si C1 116.25(6) .
N2 Si N1 82.57(5) .
C1 Si N1 93.72(6) .
N2 Si Cl 135.87(5) .
C1 Si Cl 107.34(5) .
N1 Si Cl 88.32(4) .
N2 Si S 88.67(4) .
C1 Si S 100.71(5) .
N1 Si S 165.34(4) .
Cl Si S 89.85(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.399(2) .
C1 C6 1.4010(19) .
C1 Si 1.8761(14) .
C2 C3 1.394(2) .
C3 C4 1.388(2) .
C4 C5 1.385(2) .
C5 C6 1.396(2) .
C7 N1 1.353(2) .
C7 C8 1.385(2) .
C8 C9 1.390(3) .
C9 C10 1.384(3) .
C10 C11 1.398(2) .
C11 N1 1.3444(17) .
C11 C12 1.493(2) .
C12 N2 1.4569(17) .
C13 C14 1.400(2) .
C13 N2 1.4048(19) .
C13 C18 1.4160(19) .
C14 C15 1.397(2) .
C15 C16 1.381(3) .
C16 C17 1.402(2) .
C17 C18 1.392(2) .
C18 S 1.7568(15) .
C19 C20 1.519(4) .
C20 C21 1.386(2) 2_655
C20 C21 1.386(2) .
C21 C22 1.385(3) .
C22 C23 1.389(3) .
C23 C22 1.389(3) 2_655
Cl Si 2.1430(7) .
N1 Si 1.9958(12) .
N2 Si 1.7637(12) .
S Si 2.2487(6) .
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_site_symmetry_4
C6 C1 C2 C3 -0.9(2) . .
Si C1 C2 C3 175.26(14) . .
C1 C2 C3 C4 -0.1(3) . .
C2 C3 C4 C5 1.1(3) . .
C3 C4 C5 C6 -1.0(2) . .
C4 C5 C6 C1 0.0(2) . .
C2 C1 C6 C5 0.9(2) . .
Si C1 C6 C5 -175.06(11) . .
N1 C7 C8 C9 1.5(2) . .
C7 C8 C9 C10 0.1(3) . .
C8 C9 C10 C11 -1.7(2) . .
C9 C10 C11 N1 1.9(2) . .
C9 C10 C11 C12 -178.38(15) . .
N1 C11 C12 N2 -0.54(17) . .
C10 C11 C12 N2 179.72(14) . .
N2 C13 C14 C15 179.30(14) . .
C18 C13 C14 C15 0.1(2) . .
C13 C14 C15 C16 0.2(2) . .
C14 C15 C16 C17 -0.5(2) . .
C15 C16 C17 C18 0.5(2) . .
C16 C17 C18 C13 -0.2(2) . .
C16 C17 C18 S -176.73(12) . .
C14 C13 C18 C17 -0.1(2) . .
N2 C13 C18 C17 -179.35(13) . .
C14 C13 C18 S 176.71(11) . .
N2 C13 C18 S -2.54(17) . .
C21 C20 C21 C22 -0.40(13) 2_655 .
C19 C20 C21 C22 179.61(13) . .
C20 C21 C22 C23 0.8(3) . .
C21 C22 C23 C22 -0.39(13) . 2_655
C10 C11 N1 C7 -0.3(2) . .
C12 C11 N1 C7 179.90(13) . .
C10 C11 N1 Si 175.99(12) . .
C12 C11 N1 Si -3.77(15) . .
C8 C7 N1 C11 -1.4(2) . .
C8 C7 N1 Si -177.23(12) . .
C14 C13 N2 C12 -2.0(2) . .
C18 C13 N2 C12 177.20(12) . .
C14 C13 N2 Si 173.94(11) . .
C18 C13 N2 Si -6.86(17) . .
C11 C12 N2 C13 -178.51(12) . .
C11 C12 N2 Si 5.50(16) . .
C17 C18 S Si -175.59(12) . .
C13 C18 S Si 7.73(11) . .
C13 N2 Si C1 -91.39(12) . .
C12 N2 Si C1 84.39(12) . .
C13 N2 Si N1 178.12(11) . .
C12 N2 Si N1 -6.10(11) . .
C13 N2 Si Cl 98.31(11) . .
C12 N2 Si Cl -85.91(12) . .
C13 N2 Si S 9.90(11) . .
C12 N2 Si S -174.32(10) . .
C2 C1 Si N2 -0.21(14) . .
C6 C1 Si N2 175.73(11) . .
C2 C1 Si N1 83.34(13) . .
C6 C1 Si N1 -100.72(12) . .
C2 C1 Si Cl 172.73(11) . .
C6 C1 Si Cl -11.33(13) . .
C2 C1 Si S -94.04(12) . .
C6 C1 Si S 81.90(12) . .
C11 N1 Si N2 5.46(10) . .
C7 N1 Si N2 -178.48(13) . .
C11 N1 Si C1 -110.55(10) . .
C7 N1 Si C1 65.51(13) . .
C11 N1 Si Cl 142.18(10) . .
C7 N1 Si Cl -41.76(12) . .
C11 N1 Si S 59.2(2) . .
C7 N1 Si S -124.72(16) . .
C18 S Si N2 -8.68(6) . .
C18 S Si C1 107.79(7) . .
C18 S Si N1 -61.82(17) . .
C18 S Si Cl -144.58(5) . .
