#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:07:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179880 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/76/7017660.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_7017660
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         'C19 H18 N2 S Se Si'
_chemical_formula_sum            'C19 H18 N2 S Se Si'
_chemical_formula_weight         413.46
_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                 97.973(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.5484(12)
_cell_length_b                   16.447(4)
_cell_length_c                   14.428(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      5.9
_cell_volume                     1773.9(6)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24275
_diffrn_reflns_theta_full        29.18
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    2.305
_exptl_absorpt_correction_T_max  0.4146
_exptl_absorpt_correction_T_min  0.3469
_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    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular_piece
_exptl_crystal_F_000             840
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0294
_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)+(0.0521P)²+0.0445P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                3849
_reflns_number_total             4716
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11306b.txt
_cod_data_source_block           kob17cabsu_10
_cod_original_cell_volume        1773.8(6)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7017660
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
C1 C 0.7898(3) 0.63661(14) 0.25997(14) 0.0340(4) Uani 1 1 d .
H1A H 0.7658 0.6940 0.2718 0.051 Uiso 1 1 calc R
H1B H 0.7717 0.6265 0.1924 0.051 Uiso 1 1 calc R
H1C H 0.9136 0.6236 0.2857 0.051 Uiso 1 1 calc R
C2 C 0.2578(3) 0.51621(12) 0.16942(13) 0.0271(4) Uani 1 1 d .
C3 C 0.3023(3) 0.52353(14) 0.08000(14) 0.0393(5) Uani 1 1 d .
H3 H 0.3752 0.5675 0.0653 0.047 Uiso 1 1 calc R
C4 C 0.2412(4) 0.46696(17) 0.01165(16) 0.0498(6) Uani 1 1 d .
H4 H 0.2719 0.4723 -0.0497 0.060 Uiso 1 1 calc R
C5 C 0.1366(4) 0.40343(18) 0.0327(2) 0.0570(7) Uani 1 1 d .
H5 H 0.0952 0.3646 -0.0141 0.068 Uiso 1 1 calc R
C6 C 0.0911(4) 0.39573(18) 0.1215(2) 0.0609(8) Uani 1 1 d .
H6 H 0.0186 0.3515 0.1358 0.073 Uiso 1 1 calc R
C7 C 0.1505(3) 0.45211(15) 0.19034(18) 0.0435(5) Uani 1 1 d .
H7 H 0.1180 0.4469 0.2514 0.052 Uiso 1 1 calc R
C8 C 0.5254(3) 0.73404(12) 0.39132(14) 0.0326(4) Uani 1 1 d .
H8 H 0.5069 0.7518 0.3280 0.039 Uiso 1 1 calc R
C9 C 0.4832(3) 0.78529(13) 0.45991(16) 0.0380(5) Uani 1 1 d .
H9 H 0.4349 0.8377 0.4445 0.046 Uiso 1 1 calc R
C10 C 0.5126(3) 0.75912(14) 0.55331(15) 0.0380(5) Uani 1 1 d .
H10 H 0.4819 0.7932 0.6018 0.046 Uiso 1 1 calc R
C11 C 0.5863(3) 0.68366(13) 0.57423(14) 0.0331(4) Uani 1 1 d .
H11 H 0.6099 0.6655 0.6372 0.040 Uiso 1 1 calc R
C12 C 0.6257(2) 0.63448(12) 0.50117(12) 0.0264(4) Uani 1 1 d .
C13 C 0.7066(3) 0.55182(11) 0.51369(12) 0.0260(4) Uani 1 1 d .
H13A H 0.8294 0.5556 0.5479 0.031 Uiso 1 1 calc R
H13B H 0.6345 0.5172 0.5503 0.031 Uiso 1 1 calc R
C14 C 0.7792(2) 0.43795(11) 0.41828(13) 0.0257(3) Uani 1 1 d .
C15 C 0.8544(3) 0.39407(12) 0.49733(14) 0.0311(4) Uani 1 1 d .
H15 H 0.8604 0.4176 0.5578 0.037 Uiso 1 1 calc R
C16 C 0.9204(3) 0.31595(14) 0.48709(16) 0.0388(5) Uani 1 1 d .
H16 H 0.9716 0.2865 0.5408 0.047 Uiso 1 1 calc R
C17 C 0.9119(3) 0.28078(13) 0.39907(18) 0.0419(5) Uani 1 1 d .
H17 H 0.9585 0.2277 0.3927 0.050 Uiso 1 1 calc R
C18 C 0.8353(3) 0.32311(13) 0.32059(16) 0.0357(4) Uani 1 1 d .
H18 H 0.8284 0.2988 0.2605 0.043 Uiso 1 1 calc R
C19 C 0.7686(3) 0.40111(12) 0.32954(14) 0.0289(4) Uani 1 1 d .
N2 N 0.7107(2) 0.51678(10) 0.42138(10) 0.0252(3) Uani 1 1 d .
N1 N 0.5929(2) 0.65845(9) 0.41153(11) 0.0258(3) Uani 1 1 d .
S S 0.65889(8) 0.45603(3) 0.23430(3) 0.03617(13) Uani 1 1 d .
Se Se 0.33070(3) 0.596373(12) 0.263822(13) 0.02817(7) Uani 1 1 d .
Si Si 0.63319(7) 0.57092(3) 0.31754(3) 0.02397(11) 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'
Se Se -0.0929 2.2259 '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
C3 C2 C7 119.6(2)
C3 C2 Se 121.27(16)
C7 C2 Se 119.06(15)
C2 C3 C4 120.3(2)
C5 C4 C3 120.0(2)
C4 C5 C6 120.1(2)
C5 C6 C7 120.5(3)
C6 C7 C2 119.5(2)
N1 C8 C9 121.67(19)
C8 C9 C10 118.9(2)
C11 C10 C9 119.51(19)
C10 C11 C12 118.68(19)
N1 C12 C11 121.90(19)
N1 C12 C13 113.73(16)
C11 C12 C13 124.37(17)
N2 C13 C12 108.09(15)
N2 C14 C15 124.13(17)
N2 C14 C19 116.95(16)
C15 C14 C19 118.92(18)
C16 C15 C14 119.9(2)
C17 C16 C15 120.6(2)
C18 C17 C16 120.0(2)
C17 C18 C19 120.2(2)
C18 C19 C14 120.38(18)
C18 C19 S 122.70(16)
C14 C19 S 116.85(14)
C14 N2 C13 116.82(15)
C14 N2 Si 121.27(12)
C13 N2 Si 121.91(13)
C12 N1 C8 119.27(16)
C12 N1 Si 114.26(13)
C8 N1 Si 126.28(13)
C19 S Si 94.60(7)
C2 Se Si 106.38(6)
N2 Si C1 120.60(9)
N2 Si N1 81.60(7)
C1 Si N1 92.83(8)
N2 Si S 89.23(6)
C1 Si S 98.06(7)
N1 Si S 168.34(5)
N2 Si Se 124.16(6)
C1 Si Se 113.26(7)
N1 Si Se 82.23(5)
S Si Se 97.18(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 Si 1.878(2)
C2 C3 1.383(3)
C2 C7 1.388(3)
C2 Se 1.9204(19)
C3 C4 1.387(3)
C4 C5 1.369(4)
C5 C6 1.378(5)
C6 C7 1.387(4)
C8 N1 1.360(3)
C8 C9 1.371(3)
C9 C10 1.403(3)
C10 C11 1.376(3)
C11 C12 1.393(3)
C12 N1 1.342(2)
C12 C13 1.491(3)
C13 N2 1.455(2)
C14 N2 1.399(2)
C14 C15 1.402(3)
C14 C19 1.409(3)
C15 C16 1.393(3)
C16 C17 1.389(3)
C17 C18 1.385(3)
C18 C19 1.391(3)
C19 S 1.753(2)
N2 Si 1.7709(16)
N1 Si 2.0294(16)
S Si 2.2616(8)
Se Si 2.3449(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
C7 C2 C3 C4 -0.4(4)
Se C2 C3 C4 -176.96(19)
C2 C3 C4 C5 -0.1(4)
C3 C4 C5 C6 0.3(5)
C4 C5 C6 C7 0.1(5)
C5 C6 C7 C2 -0.6(5)
C3 C2 C7 C6 0.7(4)
Se C2 C7 C6 177.4(2)
N1 C8 C9 C10 0.7(3)
C8 C9 C10 C11 1.4(3)
C9 C10 C11 C12 -1.6(3)
C10 C11 C12 N1 -0.4(3)
C10 C11 C12 C13 179.61(19)
N1 C12 C13 N2 -5.6(2)
C11 C12 C13 N2 174.41(17)
N2 C14 C15 C16 -179.55(18)
C19 C14 C15 C16 1.2(3)
C14 C15 C16 C17 -0.2(3)
C15 C16 C17 C18 -0.8(4)
C16 C17 C18 C19 0.7(4)
C17 C18 C19 C14 0.4(3)
C17 C18 C19 S -176.34(18)
N2 C14 C19 C18 179.39(18)
C15 C14 C19 C18 -1.3(3)
N2 C14 C19 S -3.7(2)
C15 C14 C19 S 175.57(14)
C15 C14 N2 C13 -4.7(3)
C19 C14 N2 C13 174.49(16)
C15 C14 N2 Si 175.18(15)
C19 C14 N2 Si -5.6(2)
C12 C13 N2 C14 -178.72(15)
C12 C13 N2 Si 1.4(2)
C11 C12 N1 C8 2.5(3)
C13 C12 N1 C8 -177.52(17)
C11 C12 N1 Si -172.81(14)
C13 C12 N1 Si 7.2(2)
C9 C8 N1 C12 -2.6(3)
C9 C8 N1 Si 172.02(16)
C18 C19 S Si -174.90(17)
C14 C19 S Si 8.28(15)
C3 C2 Se Si -77.74(18)
C7 C2 Se Si 105.66(18)
C14 N2 Si C1 -89.74(17)
C13 N2 Si C1 90.18(16)
C14 N2 Si N1 -178.06(15)
C13 N2 Si N1 1.86(14)
C14 N2 Si S 9.17(14)
C13 N2 Si S -170.91(14)
C14 N2 Si Se 107.33(13)
C13 N2 Si Se -72.75(15)
C12 N1 Si N2 -5.19(13)
C8 N1 Si N2 179.92(17)
C12 N1 Si C1 -125.72(15)
C8 N1 Si C1 59.40(18)
C12 N1 Si S 33.3(4)
C8 N1 Si S -141.6(2)
C12 N1 Si Se 121.18(13)
C8 N1 Si Se -53.70(16)
C19 S Si N2 -8.56(8)
C19 S Si C1 112.26(10)
C19 S Si N1 -46.6(3)
C19 S Si Se -132.92(7)
C2 Se Si N2 -99.06(9)
C2 Se Si C1 96.90(10)
C2 Se Si N1 -173.35(7)
C2 Se Si S -5.09(6)
