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#$Date: 2022-08-06 22:37:59 +0300 (Sat, 06 Aug 2022) $
#$Revision: 277147 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/74/1567431.cif $
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#
# 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_1567431
loop_
_publ_author_name
'Seidel, Anne'
'Weigel, Mareike'
'Ehrlich, Lisa'
'Gericke, Robert'
'Brendler, Erica'
'Wagler, Jörg'
_publ_section_title
;
 Molecular Structures of the Silicon Pyridine-2-(thi)olates Me3Si(pyX),
 Me2Si(pyX)2 and Ph2Si(pyX)2 (py = 2-Pyridyl, X = O, S), and Their Intra-
 and Intermolecular Ligand Exchange in Solution
;
_journal_issue                   8
_journal_name_full               Crystals
_journal_page_first              1054
_journal_paper_doi               10.3390/cryst12081054
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C8 H13 N S Si'
_chemical_formula_sum            'C8 H13 N S Si'
_chemical_formula_weight         183.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.954(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.6079(7)
_cell_length_b                   7.2078(6)
_cell_length_c                   11.1025(12)
_cell_measurement_reflns_used    1404
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.83
_cell_volume                     523.71(9)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7376
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         3.113
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  0.6556
_exptl_absorpt_correction_T_min  0.1135
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XShape
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       column
_exptl_crystal_F_000             196
_exptl_crystal_size_max          25
_exptl_crystal_size_mid          1.000
_exptl_crystal_size_min          1.000
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.127(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0463P)²+0.1160P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1255
_reflns_number_total             1356
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file
CIFs_all-in-one_SeidelWeigelEhrlichGerickeBrendlerWagler_pyOpyS-silanes.cif
_cod_data_source_block           pyssime3_01
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               1567431
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.039
_shelx_estimated_absorpt_t_max   0.710
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.46304(7) 0.2500 0.21454(4) 0.04784(19) Uani 1 2 d S T P . .
Si1 Si 0.74973(7) 0.2500 0.14126(4) 0.03575(18) Uani 1 2 d S T P . .
N1 N 0.7395(3) 0.2500 0.41465(15) 0.0521(4) Uani 1 2 d S T P . .
C1 C 0.5410(3) 0.2500 0.37412(16) 0.0402(4) Uani 1 2 d S T P . .
C2 C 0.3902(3) 0.2500 0.45022(19) 0.0511(5) Uani 1 2 d S T P . .
H2 H 0.2508 0.2500 0.4184 0.061 Uiso 1 2 calc R U P . .
C3 C 0.4533(4) 0.2500 0.5744(2) 0.0619(6) Uani 1 2 d S T P . .
H3 H 0.3562 0.2500 0.6288 0.074 Uiso 1 2 calc R U P . .
C4 C 0.6578(4) 0.2500 0.6177(2) 0.0642(6) Uani 1 2 d S T P . .
H4 H 0.7032 0.2500 0.7018 0.077 Uiso 1 2 calc R U P . .
C5 C 0.7937(4) 0.2500 0.5361(2) 0.0618(6) Uani 1 2 d S T P . .
H5 H 0.9338 0.2500 0.5663 0.074 Uiso 1 2 calc R U P . .
C6 C 0.8991(2) 0.0358(2) 0.18373(15) 0.0549(4) Uani 1 1 d . . . . .
H6A H 1.0251 0.0388 0.1480 0.082 Uiso 1 1 calc R U . . .
H6B H 0.8195 -0.0718 0.1538 0.082 Uiso 1 1 calc R U . . .
H6C H 0.9309 0.0285 0.2716 0.082 Uiso 1 1 calc R U . . .
C7 C 0.6590(4) 0.2500 -0.02563(18) 0.0536(5) Uani 1 2 d S T P . .
H7A H 0.6151 0.1260 -0.0513 0.080 Uiso 0.5 1 calc R U P . .
H7B H 0.7696 0.2886 -0.0691 0.080 Uiso 0.5 1 calc R U P . .
H7C H 0.5453 0.3354 -0.0432 0.080 Uiso 0.5 1 calc R U P . .
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'
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
_geom_angle_publ_flag
C1 S1 Si1 103.13(6) . . ?
C6 Si1 C6 112.41(10) . 4_565 ?
C6 Si1 C7 109.77(6) . . ?
C6 Si1 C7 109.77(6) 4_565 . ?
C6 Si1 S1 111.52(5) . . ?
C6 Si1 S1 111.52(5) 4_565 . ?
C7 Si1 S1 101.29(8) . . ?
C1 N1 C5 116.96(18) . . ?
N1 C1 C2 123.44(18) . . ?
N1 C1 S1 118.37(13) . . ?
C2 C1 S1 118.18(16) . . ?
C3 C2 C1 117.5(2) . . ?
C3 C2 H2 121.2 . . ?
C1 C2 H2 121.2 . . ?
C4 C3 C2 119.8(2) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C4 C3 118.4(2) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
N1 C5 C4 123.9(2) . . ?
N1 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.7754(19) . ?
S1 Si1 2.1627(6) . ?
Si1 C6 1.8581(15) . ?
Si1 C6 1.8581(15) 4_565 ?
Si1 C7 1.867(2) . ?
N1 C1 1.327(2) . ?
N1 C5 1.346(3) . ?
C1 C2 1.393(3) . ?
C2 C3 1.384(3) . ?
C2 H2 0.9400 . ?
C3 C4 1.370(4) . ?
C3 H3 0.9400 . ?
C4 C5 1.362(3) . ?
C4 H4 0.9400 . ?
C5 H5 0.9400 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 0.000(1) . . . . ?
C5 N1 C1 S1 180.000(0) . . . . ?
Si1 S1 C1 N1 0.000(0) . . . . ?
Si1 S1 C1 C2 180.000(0) . . . . ?
N1 C1 C2 C3 0.000(1) . . . . ?
S1 C1 C2 C3 180.000(1) . . . . ?
C1 C2 C3 C4 0.000(1) . . . . ?
C2 C3 C4 C5 0.000(1) . . . . ?
C1 N1 C5 C4 0.000(1) . . . . ?
C3 C4 C5 N1 0.000(1) . . . . ?
