#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/76/7017653.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_7017653
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(C19 H15 N3 O S Si), C7 H8'
_chemical_formula_sum            'C22.5 H19 N3 O S Si'
_chemical_formula_weight         407.56
_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                 118.544(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.439(4)
_cell_length_b                   12.6603(18)
_cell_length_c                   16.963(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      7.75
_cell_volume                     4044.5(12)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_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            31456
_diffrn_reflns_theta_full        29.14
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .25
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         5407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0452
_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)+(0.0632P)²+2.4713P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                4022
_reflns_number_total             5407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11306b.txt
_cod_data_source_block           kob06d_3
_cod_original_cell_volume        4044.5(10)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C22.50 H19 N3 O S Si'
_cod_database_code               7017653
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 0.15764(8) 1.04898(13) 0.10132(11) 0.0305(3) Uani 1 1 d .
C2 C 0.17241(9) 1.11125(13) 0.17668(11) 0.0345(3) Uani 1 1 d .
H2 H 0.2171 1.1045 0.2292 0.041 Uiso 1 1 calc R
C3 C 0.12270(11) 1.18274(14) 0.17572(13) 0.0409(4) Uani 1 1 d .
H3 H 0.1336 1.2239 0.2275 0.049 Uiso 1 1 calc R
C4 C 0.05756(11) 1.19422(15) 0.09978(15) 0.0446(4) Uani 1 1 d .
H4 H 0.0236 1.2428 0.0993 0.054 Uiso 1 1 calc R
C5 C 0.04227(10) 1.13408(17) 0.02433(15) 0.0483(5) Uani 1 1 d .
H5 H -0.0023 1.1418 -0.0282 0.058 Uiso 1 1 calc R
C6 C 0.09195(9) 1.06230(16) 0.02516(13) 0.0414(4) Uani 1 1 d .
H6 H 0.0808 1.0218 -0.0271 0.050 Uiso 1 1 calc R
C7 C 0.14925(9) 0.73673(14) 0.06499(12) 0.0354(3) Uani 1 1 d .
C8 C 0.11251(10) 0.64305(15) 0.05739(15) 0.0445(4) Uani 1 1 d .
H8 H 0.1093 0.6166 0.1077 0.053 Uiso 1 1 calc R
C9 C 0.08053(10) 0.58795(16) -0.02359(16) 0.0500(5) Uani 1 1 d .
H9 H 0.0556 0.5241 -0.0286 0.060 Uiso 1 1 calc R
C10 C 0.08541(10) 0.62703(17) -0.09673(16) 0.0489(5) Uani 1 1 d .
H10 H 0.0638 0.5894 -0.1519 0.059 Uiso 1 1 calc R
C11 C 0.12146(10) 0.72031(16) -0.09058(13) 0.0419(4) Uani 1 1 d .
H11 H 0.1241 0.7460 -0.1415 0.050 Uiso 1 1 calc R
C12 C 0.15397(8) 0.77690(14) -0.00996(11) 0.0329(3) Uani 1 1 d .
C13 C 0.19945(9) 0.91140(15) -0.07243(11) 0.0365(4) Uani 1 1 d .
H13A H 0.1523 0.9271 -0.1240 0.044 Uiso 1 1 calc R
H13B H 0.2232 0.8578 -0.0914 0.044 Uiso 1 1 calc R
C14 C 0.24313(9) 1.00936(15) -0.04243(12) 0.0374(4) Uani 1 1 d .
C15 C 0.26520(12) 1.06854(17) -0.09444(16) 0.0502(5) Uani 1 1 d .
H15 H 0.2509 1.0492 -0.1548 0.060 Uiso 1 1 calc R
C16 C 0.30791(13) 1.15518(19) -0.05666(18) 0.0592(6) Uani 1 1 d .
H16 H 0.3240 1.1957 -0.0906 0.071 Uiso 1 1 calc R
C17 C 0.32737(12) 1.18320(17) 0.03111(18) 0.0550(6) Uani 1 1 d .
H17 H 0.3573 1.2424 0.0581 0.066 Uiso 1 1 calc R
C18 C 0.30259(10) 1.12369(16) 0.07865(15) 0.0452(4) Uani 1 1 d .
H18 H 0.3146 1.1439 0.1382 0.054 Uiso 1 1 calc R
C19 C 0.35925(9) 0.95294(13) 0.25834(12) 0.0364(4) Uani 1 1 d .
C20 C 0.5000 0.1486(3) 0.2500 0.0928(15) Uani 1 2 d S
H20A H 0.5079 0.1228 0.3085 0.139 Uiso 0.50 1 calc PR
H20B H 0.5380 0.1228 0.2385 0.139 Uiso 0.50 1 calc PR
H20C H 0.4541 0.1228 0.2030 0.139 Uiso 0.50 1 calc PR
C21 C 0.5000 0.2681(3) 0.2500 0.0506(7) Uani 1 2 d S
C22 C 0.54378(12) 0.3241(2) 0.22662(16) 0.0583(6) Uani 1 1 d .
H22 H 0.5747 0.2868 0.2109 0.070 Uiso 1 1 calc R
C23 C 0.54392(14) 0.4323(2) 0.22554(17) 0.0648(7) Uani 1 1 d .
H23 H 0.5740 0.4690 0.2081 0.078 Uiso 1 1 calc R
C24 C 0.5000 0.4883(3) 0.2500 0.0689(10) Uani 1 2 d S
H24 H 0.5000 0.5633 0.2500 0.083 Uiso 1 2 calc SR
N1 N 0.26166(7) 1.03747(12) 0.04245(10) 0.0348(3) Uani 1 1 d .
N2 N 0.19139(7) 0.87175(11) 0.00299(9) 0.0319(3) Uani 1 1 d .
N3 N 0.30100(8) 0.96634(14) 0.20333(10) 0.0434(4) Uani 1 1 d .
O O 0.41783(8) 0.94243(15) 0.31509(13) 0.0756(6) Uani 1 1 d .
S S 0.19458(3) 0.80847(4) 0.16496(3) 0.04017(13) Uani 1 1 d .
Si Si 0.22099(2) 0.94613(4) 0.10261(3) 0.02981(12) 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'
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'
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
C6 C1 C2 117.69(15) . .
C6 C1 Si 120.04(13) . .
C2 C1 Si 122.20(12) . .
C3 C2 C1 121.08(17) . .
C4 C3 C2 120.40(17) . .
C3 C4 C5 119.34(17) . .
C4 C5 C6 120.37(18) . .
C1 C6 C5 121.11(18) . .
C8 C7 C12 120.09(18) . .
C8 C7 S 123.90(15) . .
C12 C7 S 115.97(13) . .
C9 C8 C7 120.43(19) . .
C10 C9 C8 119.46(19) . .
C9 C10 C11 120.95(19) . .
C10 C11 C12 120.57(19) . .
C11 C12 N2 124.90(16) . .
C11 C12 C7 118.51(17) . .
N2 C12 C7 116.59(15) . .
N2 C13 C14 107.77(14) . .
N1 C14 C15 121.10(19) . .
N1 C14 C13 113.69(14) . .
C15 C14 C13 125.21(18) . .
C16 C15 C14 118.9(2) . .
C15 C16 C17 119.74(19) . .
C18 C17 C16 119.0(2) . .
N1 C18 C17 121.5(2) . .
N3 C19 O 177.8(2) . .
C22 C21 C22 118.0(3) . 2_655
C22 C21 C20 120.99(16) . .
C22 C21 C20 120.99(16) 2_655 .
C23 C22 C21 121.7(2) . .
C22 C23 C24 120.0(2) . .
C23 C24 C23 118.7(3) . 2_655
C14 N1 C18 119.72(16) . .
C14 N1 Si 114.57(12) . .
C18 N1 Si 125.67(14) . .
C12 N2 C13 117.12(14) . .
C12 N2 Si 121.58(11) . .
C13 N2 Si 121.09(12) . .
C19 N3 Si 158.55(16) . .
C7 S Si 95.42(6) . .
N2 Si N3 137.79(7) . .
N2 Si C1 115.61(7) . .
N3 Si C1 105.89(8) . .
N2 Si N1 82.23(7) . .
N3 Si N1 87.20(7) . .
C1 Si N1 94.74(7) . .
N2 Si S 88.89(5) . .
N3 Si S 90.21(6) . .
C1 Si S 101.55(5) . .
N1 Si S 163.59(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.394(2) .
C1 C2 1.403(2) .
C1 Si 1.8740(16) .
C2 C3 1.392(2) .
C3 C4 1.383(3) .
C4 C5 1.387(3) .
C5 C6 1.395(3) .
C7 C8 1.395(3) .
C7 C12 1.417(2) .
C7 S 1.7521(19) .
C8 C9 1.394(3) .
C9 C10 1.385(3) .
C10 C11 1.388(3) .
C11 C12 1.399(2) .
C12 N2 1.402(2) .
C13 N2 1.460(2) .
C13 C14 1.490(3) .
C14 N1 1.346(2) .
C14 C15 1.401(2) .
C15 C16 1.375(3) .
C16 C17 1.387(4) .
C17 C18 1.382(3) .
C18 N1 1.350(2) .
C19 N3 1.160(2) .
C19 O 1.169(2) .
C20 C21 1.513(5) .
C21 C22 1.377(3) .
C21 C22 1.377(3) 2_655
C22 C23 1.370(4) .
C23 C24 1.391(3) .
C24 C23 1.391(3) 2_655
N1 Si 1.9972(15) .
N2 Si 1.7664(15) .
N3 Si 1.7681(17) .
S Si 2.2469(7) .
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 -176.15(13) . .
C1 C2 C3 C4 -0.4(3) . .
C2 C3 C4 C5 -0.3(3) . .
C3 C4 C5 C6 0.4(3) . .
C2 C1 C6 C5 -0.8(3) . .
Si C1 C6 C5 176.30(16) . .
C4 C5 C6 C1 0.2(3) . .
C12 C7 C8 C9 0.4(3) . .
S C7 C8 C9 -176.98(14) . .
C7 C8 C9 C10 -0.1(3) . .
C8 C9 C10 C11 -0.2(3) . .
C9 C10 C11 C12 0.2(3) . .
C10 C11 C12 N2 -179.86(16) . .
C10 C11 C12 C7 0.1(2) . .
C8 C7 C12 C11 -0.3(2) . .
S C7 C12 C11 177.20(12) . .
C8 C7 C12 N2 179.58(14) . .
S C7 C12 N2 -2.88(19) . .
N2 C13 C14 N1 -1.86(19) . .
N2 C13 C14 C15 177.17(16) . .
N1 C14 C15 C16 1.6(3) . .
C13 C14 C15 C16 -177.37(18) . .
C14 C15 C16 C17 -1.0(3) . .
C15 C16 C17 C18 -0.7(3) . .
C16 C17 C18 N1 1.9(3) . .
C22 C21 C22 C23 -0.59(18) 2_655 .
C20 C21 C22 C23 179.41(18) . .
C21 C22 C23 C24 1.2(4) . .
C22 C23 C24 C23 -0.57(17) . 2_655
C15 C14 N1 C18 -0.4(2) . .
C13 C14 N1 C18 178.62(15) . .
C15 C14 N1 Si 177.36(14) . .
C13 C14 N1 Si -3.57(18) . .
C17 C18 N1 C14 -1.3(3) . .
C17 C18 N1 Si -178.87(14) . .
C11 C12 N2 C13 -2.9(2) . .
C7 C12 N2 C13 177.23(14) . .
C11 C12 N2 Si 171.87(13) . .
C7 C12 N2 Si -8.04(19) . .
C14 C13 N2 C12 -177.61(13) . .
C14 C13 N2 Si 7.64(18) . .
O C19 N3 Si 172(100) . .
C8 C7 S Si -173.61(14) . .
C12 C7 S Si 8.96(12) . .
C12 N2 Si N3 100.65(15) . .
C13 N2 Si N3 -84.83(16) . .
C12 N2 Si C1 -90.73(13) . .
C13 N2 Si C1 83.79(13) . .
C12 N2 Si N1 177.72(13) . .
C13 N2 Si N1 -7.77(12) . .
C12 N2 Si S 11.56(12) . .
C13 N2 Si S -173.93(12) . .
C19 N3 Si N2 -11.1(5) . .
C19 N3 Si C1 179.6(4) . .
C19 N3 Si N1 -86.3(4) . .
C19 N3 Si S 77.5(4) . .
C6 C1 Si N2 0.33(17) . .
C2 C1 Si N2 177.31(12) . .
C6 C1 Si N3 172.40(14) . .
C2 C1 Si N3 -10.62(16) . .
C6 C1 Si N1 83.97(15) . .
C2 C1 Si N1 -99.04(14) . .
C6 C1 Si S -94.04(14) . .
C2 C1 Si S 82.95(14) . .
C14 N1 Si N2 6.23(12) . .
C18 N1 Si N2 -176.11(15) . .
C14 N1 Si N3 145.27(13) . .
C18 N1 Si N3 -37.07(15) . .
C14 N1 Si C1 -109.01(12) . .
C18 N1 Si C1 68.65(15) . .
C14 N1 Si S 64.1(2) . .
C18 N1 Si S -118.26(19) . .
C7 S Si N2 -10.09(7) . .
C7 S Si N3 -147.89(8) . .
C7 S Si C1 105.84(8) . .
C7 S Si N1 -67.13(19) . .
