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#$Date: 2024-01-06 21:09:52 +0200 (Sat, 06 Jan 2024) $
#$Revision: 288922 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/07/1570713.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_1570713
loop_
_publ_author_name
'Riedel, Sophie'
'Gerwig, Maik'
'Gerlach, Daniela'
'Brendler, Erica'
'Gericke, Robert'
'Kroke, Edwin'
'Wagler, Jörg'
_publ_section_title
;
 The Hexacoordinate Si Complex SiCl4(4-Azidopyridine)2---Crystallographic
 Characterization of Two Conformers and Probing the Influence of
 SiCl4-Complexation on a Click Reaction with Phenylacetylene
;
_journal_issue                   12
_journal_name_full               Inorganics
_journal_page_first              473
_journal_paper_doi               10.3390/inorganics11120473
_journal_volume                  11
_journal_year                    2023
_chemical_formula_moiety         'C10 H8 Cl4 N8 Si'
_chemical_formula_sum            'C10 H8 Cl4 N8 Si'
_chemical_formula_weight         410.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ShelXT
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 94.795(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.2920(6)
_cell_length_b                   10.7627(6)
_cell_length_c                   10.0442(8)
_cell_measurement_reflns_used    13749
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.78
_cell_volume                     785.53(10)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0224
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12304
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.992
_diffrn_reflns_theta_min         2.779
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.9221
_exptl_absorpt_correction_T_min  0.7556
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XShape
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       piece
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0102(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.277
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0207P)²+0.7118P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1671
_reflns_number_total             1895
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            all-in-one.cif
_cod_data_source_block           compound-2-prime
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1570713
_shelx_shelxl_version_number     2018/3
_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   0.709
_shelx_estimated_absorpt_t_max   0.850
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_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
Cl1 Cl 0.39773(6) -0.02162(5) 0.29044(4) 0.02948(14) Uani 1 1 d . . . . .
Cl2 Cl 0.23399(6) 0.07545(4) 0.54930(5) 0.02942(14) Uani 1 1 d . . . . .
Si1 Si 0.500000 0.000000 0.500000 0.02188(16) Uani 1 2 d S . P . .
C1 C 0.7524(2) 0.21047(18) 0.51043(18) 0.0256(4) Uani 1 1 d . . . . .
H1 H 0.832633 0.154807 0.560188 0.031 Uiso 1 1 calc R U . . .
N1 N 0.5851(2) 0.16884(15) 0.46170(15) 0.0235(3) Uani 1 1 d . . . . .
N2 N 0.7566(2) 0.53481(16) 0.40356(19) 0.0325(4) Uani 1 1 d . . . . .
N3 N 0.6479(3) 0.60241(16) 0.33190(18) 0.0339(4) Uani 1 1 d . . . . .
N4 N 0.5620(3) 0.67185(19) 0.2709(2) 0.0492(5) Uani 1 1 d . . . . .
C2 C 0.8114(3) 0.33046(19) 0.4909(2) 0.0285(4) Uani 1 1 d . . . . .
H2 H 0.929426 0.356795 0.527295 0.034 Uiso 1 1 calc R U . . .
C3 C 0.6956(3) 0.41202(17) 0.41737(18) 0.0255(4) Uani 1 1 d . . . . .
C4 C 0.5244(3) 0.36905(18) 0.36421(19) 0.0276(4) Uani 1 1 d . . . . .
H4 H 0.443547 0.422391 0.311827 0.033 Uiso 1 1 calc R U . . .
C5 C 0.4742(2) 0.24857(18) 0.38851(19) 0.0267(4) Uani 1 1 d . . . . .
H5 H 0.357027 0.220175 0.352498 0.032 Uiso 1 1 calc R U . . .
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'
Cl Cl 0.1484 0.1585 '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'
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
N1 Si1 N1 180.0 3_656 . ?
N1 Si1 Cl1 89.88(5) 3_656 3_656 ?
N1 Si1 Cl1 90.13(5) . 3_656 ?
N1 Si1 Cl1 90.12(5) 3_656 . ?
N1 Si1 Cl1 89.87(5) . . ?
Cl1 Si1 Cl1 180.0 3_656 . ?
N1 Si1 Cl2 89.92(5) 3_656 . ?
N1 Si1 Cl2 90.08(5) . . ?
Cl1 Si1 Cl2 88.865(19) 3_656 . ?
Cl1 Si1 Cl2 91.134(19) . . ?
N1 Si1 Cl2 90.08(5) 3_656 3_656 ?
N1 Si1 Cl2 89.92(5) . 3_656 ?
Cl1 Si1 Cl2 91.134(19) 3_656 3_656 ?
Cl1 Si1 Cl2 88.867(19) . 3_656 ?
Cl2 Si1 Cl2 180.0 . 3_656 ?
N1 C1 C2 122.76(17) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C1 N1 C5 117.81(16) . . ?
C1 N1 Si1 121.65(13) . . ?
C5 N1 Si1 120.52(12) . . ?
N3 N2 C3 114.28(17) . . ?
N4 N3 N2 173.4(2) . . ?
C1 C2 C3 118.98(17) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C2 C3 C4 118.64(17) . . ?
C2 C3 N2 117.65(17) . . ?
C4 C3 N2 123.69(18) . . ?
C5 C4 C3 119.21(18) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 122.58(17) . . ?
N1 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
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
Cl1 Si1 2.1859(5) . ?
Cl2 Si1 2.1972(5) . ?
Si1 N1 1.9685(15) 3_656 ?
Si1 N1 1.9685(15) . ?
C1 N1 1.352(2) . ?
C1 C2 1.380(3) . ?
C1 H1 0.9500 . ?
N1 C5 1.353(2) . ?
N2 N3 1.257(3) . ?
N2 C3 1.405(2) . ?
N3 N4 1.123(3) . ?
C2 C3 1.387(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.394(3) . ?
C4 C5 1.375(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
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
C2 C1 N1 C5 1.5(3) . . . . ?
C2 C1 N1 Si1 -176.49(14) . . . . ?
N1 C1 C2 C3 -0.6(3) . . . . ?
C1 C2 C3 C4 -0.9(3) . . . . ?
C1 C2 C3 N2 177.61(17) . . . . ?
N3 N2 C3 C2 177.62(18) . . . . ?
N3 N2 C3 C4 -4.0(3) . . . . ?
C2 C3 C4 C5 1.4(3) . . . . ?
N2 C3 C4 C5 -177.02(18) . . . . ?
C1 N1 C5 C4 -0.9(3) . . . . ?
Si1 N1 C5 C4 177.04(15) . . . . ?
C3 C4 C5 N1 -0.5(3) . . . . ?
