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#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/76/7017652.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_7017652
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 Br N2 S Si), C7 H8'
_chemical_formula_sum            'C21.5 H19 Br N2 S Si'
_chemical_formula_weight         445.45
_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                 121.25(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.133(4)
_cell_length_b                   12.662(3)
_cell_length_c                   17.279(4)
_cell_measurement_reflns_used    3213
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.75
_cell_measurement_theta_min      8.25
_cell_volume                     3953(2)
_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 0.942
_diffrn_measured_fraction_theta_max 0.942
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0382
_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            26240
_diffrn_reflns_theta_full        29.11
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    2.255
_exptl_absorpt_correction_T_max  0.3993
_exptl_absorpt_correction_T_min  0.3656
_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    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       long_prism
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0317
_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)+(0.0494P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                3768
_reflns_number_total             4998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11306b.txt
_cod_data_source_block           kob05l_2
_cod_original_cell_volume        3952.5(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C21.50 H19 Br N2 S Si'
_cod_database_code               7017652
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
Br Br 0.163848(11) 0.954879(17) 0.263575(15) 0.02668(7) Uani 1 1 d .
C1 C 0.33899(10) 1.04656(16) 0.39901(15) 0.0212(4) Uani 1 1 d .
C2 C 0.32295(11) 1.10544(16) 0.32284(16) 0.0240(4) Uani 1 1 d .
H2 H 0.2764 1.0965 0.2686 0.030(7) Uiso 1 1 calc R
C3 C 0.37384(13) 1.17745(17) 0.32442(18) 0.0284(5) Uani 1 1 d .
H3 H 0.3617 1.2169 0.2717 0.038(7) Uiso 1 1 calc R
C4 C 0.44190(13) 1.19095(19) 0.40292(19) 0.0340(5) Uani 1 1 d .
H4 H 0.4770 1.2387 0.4040 0.045(8) Uiso 1 1 calc R
C5 C 0.45845(13) 1.1348(2) 0.4795(2) 0.0432(7) Uani 1 1 d .
H5 H 0.5048 1.1450 0.5338 0.057(9) Uiso 1 1 calc R
C6 C 0.40745(13) 1.0627(2) 0.47787(18) 0.0360(6) Uani 1 1 d .
H6 H 0.4196 1.0243 0.5311 0.054(9) Uiso 1 1 calc R
C7 C 0.19581(12) 1.11988(18) 0.42225(18) 0.0293(5) Uani 1 1 d .
H7 H 0.1823 1.1412 0.3629 0.030(7) Uiso 1 1 calc R
C8 C 0.17335(13) 1.18031(19) 0.47041(19) 0.0343(6) Uani 1 1 d .
H8 H 0.1439 1.2416 0.4441 0.032(7) Uiso 1 1 calc R
C9 C 0.19464(14) 1.1499(2) 0.5582(2) 0.0373(6) Uani 1 1 d .
H9 H 0.1797 1.1901 0.5924 0.039(7) Uiso 1 1 calc R
C10 C 0.23764(14) 1.06091(19) 0.59481(19) 0.0326(5) Uani 1 1 d .
H10 H 0.2537 1.0400 0.6551 0.045(8) Uiso 1 1 calc R
C11 C 0.25732(11) 1.00175(17) 0.54216(15) 0.0234(4) Uani 1 1 d .
C12 C 0.30275(11) 0.90313(17) 0.57307(15) 0.0242(4) Uani 1 1 d .
H12A H 0.3518 0.9178 0.6273 0.028(6) Uiso 1 1 calc R
H12B H 0.2777 0.8487 0.5889 0.024(6) Uiso 1 1 calc R
C13 C 0.35141(11) 0.77173(16) 0.51362(16) 0.0227(4) Uani 1 1 d .
C14 C 0.38574(12) 0.71465(18) 0.59489(17) 0.0288(5) Uani 1 1 d .
H14 H 0.3828 0.7394 0.6449 0.044(8) Uiso 1 1 calc R
C15 C 0.42413(13) 0.62179(18) 0.60286(19) 0.0348(6) Uani 1 1 d .
H15 H 0.4472 0.5838 0.6583 0.040(8) Uiso 1 1 calc R
C16 C 0.42895(13) 0.58430(18) 0.5306(2) 0.0349(6) Uani 1 1 d .
H16 H 0.4556 0.5213 0.5368 0.028(6) Uiso 1 1 calc R
C17 C 0.39449(12) 0.63951(18) 0.44885(18) 0.0307(5) Uani 1 1 d .
H17 H 0.3971 0.6135 0.3990 0.037(7) Uiso 1 1 calc R
C18 C 0.35611(11) 0.73302(16) 0.44001(16) 0.0237(4) Uani 1 1 d .
C19 C 0.0000 1.1426(3) 0.2500 0.0623(14) Uani 1 2 d S
H19A H 0.0016 1.1168 0.3044 0.094 Uiso 0.50 1 calc PR
H19B H 0.0435 1.1168 0.2494 0.094 Uiso 0.50 1 calc PR
H19C H -0.0451 1.1168 0.1961 0.094 Uiso 0.50 1 calc PR
C20 C 0.0000 1.2623(3) 0.2500 0.0356(8) Uani 1 2 d S
C21 C 0.04506(14) 1.3189(2) 0.2287(2) 0.0415(6) Uani 1 1 d .
H21 H 0.0767 1.2818 0.2143 0.050 Uiso 1 1 calc R
C22 C 0.04506(16) 1.4278(3) 0.2278(2) 0.0504(8) Uani 1 1 d .
H22 H 0.0759 1.4649 0.2121 0.060 Uiso 1 1 calc R
C23 C 0.0000 1.4830(3) 0.2500 0.0548(12) Uani 1 2 d S
H23 H 0.0000 1.5581 0.2500 0.066 Uiso 1 2 calc SR
N1 N 0.23678(9) 1.03079(13) 0.45777(13) 0.0225(4) Uani 1 1 d .
N2 N 0.31130(9) 0.86601(13) 0.49919(12) 0.0215(4) Uani 1 1 d .
S S 0.30713(3) 0.80522(4) 0.33927(4) 0.02833(13) Uani 1 1 d .
Si Si 0.27704(3) 0.93991(4) 0.39885(4) 0.01945(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'
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'
Br Br -0.2901 2.4595 '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
C2 C1 C6 117.74(19) . .
C2 C1 Si 123.72(16) . .
C6 C1 Si 118.36(17) . .
C1 C2 C3 121.5(2) . .
C4 C3 C2 119.8(2) . .
C5 C4 C3 119.6(2) . .
C4 C5 C6 120.5(2) . .
C1 C6 C5 120.8(2) . .
N1 C7 C8 121.6(2) . .
C7 C8 C9 118.9(2) . .
C10 C9 C8 119.3(2) . .
C9 C10 C11 119.1(2) . .
N1 C11 C10 121.6(2) . .
N1 C11 C12 113.81(18) . .
C10 C11 C12 124.6(2) . .
N2 C12 C11 107.77(18) . .
C14 C13 N2 124.4(2) . .
C14 C13 C18 118.8(2) . .
N2 C13 C18 116.80(19) . .
C15 C14 C13 120.4(2) . .
C16 C15 C14 120.7(2) . .
C15 C16 C17 119.7(2) . .
C16 C17 C18 120.2(2) . .
C17 C18 C13 120.2(2) . .
C17 C18 S 124.11(19) . .
C13 C18 S 115.60(16) . .
C21 C20 C21 117.7(4) . 2
C21 C20 C19 121.14(18) . .
C21 C20 C19 121.14(18) 2 .
C22 C21 C20 121.6(3) . .
C21 C22 C23 119.8(3) . .
C22 C23 C22 119.4(4) 2 .
C11 N1 C7 119.36(19) . .
C11 N1 Si 114.46(14) . .
C7 N1 Si 126.04(16) . .
C13 N2 C12 117.06(18) . .
C13 N2 Si 121.76(14) . .
C12 N2 Si 121.10(14) . .
C18 S Si 95.88(8) . .
N2 Si C1 116.73(9) . .
N2 Si N1 82.56(8) . .
C1 Si N1 93.78(8) . .
N2 Si S 88.76(6) . .
C1 Si S 100.56(7) . .
N1 Si S 165.45(6) . .
N2 Si Br 135.64(6) . .
C1 Si Br 107.16(7) . .
N1 Si Br 88.70(6) . .
S Si Br 89.39(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br Si 2.3280(13) .
C1 C2 1.393(3) .
C1 C6 1.395(3) .
C1 Si 1.880(2) .
C2 C3 1.399(3) .
C3 C4 1.383(4) .
C4 C5 1.378(4) .
C5 C6 1.402(3) .
C7 N1 1.359(3) .
C7 C8 1.383(3) .
C8 C9 1.393(4) .
C9 C10 1.378(4) .
C10 C11 1.398(3) .
C11 N1 1.339(3) .
C11 C12 1.495(3) .
C12 N2 1.457(3) .
C13 C14 1.401(3) .
C13 N2 1.409(3) .
C13 C18 1.414(3) .
C14 C15 1.394(3) .
C15 C16 1.388(4) .
C16 C17 1.395(4) .
C17 C18 1.398(3) .
C18 S 1.751(2) .
C19 C20 1.516(5) .
C20 C21 1.385(3) .
C20 C21 1.385(3) 2
C21 C22 1.379(4) .
C22 C23 1.386(4) .
C23 C22 1.386(4) 2
N1 Si 1.9958(18) .
N2 Si 1.7616(19) .
S Si 2.2477(8) .
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 0.8(3) . .
Si C1 C2 C3 -174.25(16) . .
C1 C2 C3 C4 0.2(3) . .
C2 C3 C4 C5 -1.2(4) . .
C3 C4 C5 C6 1.2(4) . .
C2 C1 C6 C5 -0.9(4) . .
Si C1 C6 C5 174.5(2) . .
C4 C5 C6 C1 -0.1(4) . .
N1 C7 C8 C9 1.3(3) . .
C7 C8 C9 C10 0.2(3) . .
C8 C9 C10 C11 -1.6(3) . .
C9 C10 C11 N1 1.5(3) . .
C9 C10 C11 C12 -179.2(2) . .
N1 C11 C12 N2 -0.3(2) . .
C10 C11 C12 N2 -179.63(19) . .
N2 C13 C14 C15 179.80(19) . .
C18 C13 C14 C15 0.4(3) . .
C13 C14 C15 C16 -0.1(3) . .
C14 C15 C16 C17 -0.6(3) . .
C15 C16 C17 C18 0.9(3) . .
C16 C17 C18 C13 -0.6(3) . .
C16 C17 C18 S -176.78(17) . .
C14 C13 C18 C17 -0.1(3) . .
N2 C13 C18 C17 -179.53(17) . .
C14 C13 C18 S 176.45(15) . .
N2 C13 C18 S -3.0(2) . .
C21 C20 C21 C22 -0.5(2) 2 .
C19 C20 C21 C22 179.5(2) . .
C20 C21 C22 C23 1.0(4) . .
C21 C22 C23 C22 -0.5(2) . 2
C10 C11 N1 C7 0.0(3) . .
C12 C11 N1 C7 -179.39(18) . .
C10 C11 N1 Si 175.99(16) . .
C12 C11 N1 Si -3.4(2) . .
C8 C7 N1 C11 -1.4(3) . .
C8 C7 N1 Si -176.90(16) . .
C14 C13 N2 C12 -2.8(3) . .
C18 C13 N2 C12 176.66(16) . .
C14 C13 N2 Si 173.96(15) . .
C18 C13 N2 Si -6.6(2) . .
C11 C12 N2 C13 -178.67(16) . .
C11 C12 N2 Si 4.6(2) . .
C17 C18 S Si -175.48(17) . .
C13 C18 S Si 8.16(15) . .
C13 N2 Si C1 -91.27(17) . .
C12 N2 Si C1 85.31(16) . .
C13 N2 Si N1 178.23(16) . .
C12 N2 Si N1 -5.19(15) . .
C13 N2 Si S 9.94(15) . .
C12 N2 Si S -173.48(14) . .
C13 N2 Si Br 97.79(15) . .
C12 N2 Si Br -85.62(16) . .
C2 C1 Si N2 174.08(16) . .
C6 C1 Si N2 -1.0(2) . .
C2 C1 Si N1 -102.35(18) . .
C6 C1 Si N1 82.58(19) . .
C2 C1 Si S 80.11(18) . .
C6 C1 Si S -94.96(18) . .
C2 C1 Si Br -12.54(19) . .
C6 C1 Si Br 172.38(17) . .
C11 N1 Si N2 4.75(14) . .
C7 N1 Si N2 -179.56(17) . .
C11 N1 Si C1 -111.73(15) . .
C7 N1 Si C1 63.95(18) . .
C11 N1 Si S 58.6(3) . .
C7 N1 Si S -125.7(2) . .
C11 N1 Si Br 141.16(13) . .
C7 N1 Si Br -43.16(16) . .
C18 S Si N2 -8.94(8) . .
C18 S Si C1 108.03(10) . .
C18 S Si N1 -62.2(3) . .
C18 S Si Br -144.62(7) . .
