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#$Date: 2024-01-06 20:09:52 +0100 (sáb 06 de ene de 2024) $
#$Revision: 288922 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/07/1570716.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_1570716
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         'C13 H10 N4'
_chemical_formula_sum            'C13 H10 N4'
_chemical_formula_weight         222.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ShelXT
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                75.071(6)
_cell_angle_beta                 79.636(6)
_cell_angle_gamma                89.686(6)
_cell_formula_units_Z            2
_cell_length_a                   5.6770(4)
_cell_length_b                   7.1648(5)
_cell_length_c                   13.4102(11)
_cell_measurement_reflns_used    8155
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      3.65
_cell_volume                     517.96(7)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       'onmega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7244
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.989
_diffrn_reflns_theta_min         1.599
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       needle
_exptl_crystal_F_000             232
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.14(2)
_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   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         7244
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0488
_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)+(0.0780P)²+0.0403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5459
_reflns_number_total             7244
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            all-in-one.cif
_cod_data_source_block           compound-1,4-3
_cod_database_code               1570716
_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   0.915
_shelx_estimated_absorpt_t_max   0.996
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
N1 N 0.3879(3) 0.8292(2) 0.41758(14) 0.0221(4) Uani 1 1 d . . . . .
N2 N 0.6047(3) 0.8086(3) 0.44748(14) 0.0269(5) Uani 1 1 d . . . . .
N3 N 0.5656(4) 0.7146(3) 0.54710(15) 0.0275(5) Uani 1 1 d . . . . .
N4 N 0.3483(4) 1.1243(3) 0.10634(15) 0.0299(5) Uani 1 1 d . . . . .
C1 C 0.3253(4) 0.6742(3) 0.58191(17) 0.0202(5) Uani 1 1 d . . . . .
C2 C 0.2105(4) 0.7475(3) 0.49933(17) 0.0219(4) Uani 1 1 d . . . . .
H2 H 0.043319 0.742155 0.499433 0.026 Uiso 1 1 calc R U . . .
C3 C 0.5424(4) 1.0279(3) 0.13069(18) 0.0287(5) Uani 1 1 d . . . . .
H3 H 0.672644 1.027316 0.075283 0.034 Uiso 1 1 calc R U . . .
C4 C 0.5641(4) 0.9291(3) 0.23201(17) 0.0248(5) Uani 1 1 d . . . . .
H4 H 0.705271 0.863388 0.245832 0.030 Uiso 1 1 calc R U . . .
C5 C 0.3736(4) 0.9297(3) 0.31199(16) 0.0211(5) Uani 1 1 d . . . . .
C6 C 0.1701(4) 1.0258(3) 0.29004(16) 0.0242(5) Uani 1 1 d . . . . .
H6 H 0.036732 1.026646 0.344048 0.029 Uiso 1 1 calc R U . . .
C7 C 0.1675(4) 1.1210(3) 0.18623(18) 0.0278(5) Uani 1 1 d . . . . .
H7 H 0.028376 1.188317 0.170744 0.033 Uiso 1 1 calc R U . . .
C8 C 0.2279(4) 0.5697(3) 0.69023(16) 0.0218(5) Uani 1 1 d . . . . .
C9 C 0.3611(4) 0.5646(3) 0.76904(17) 0.0244(5) Uani 1 1 d . . . . .
H9 H 0.514127 0.629711 0.751825 0.029 Uiso 1 1 calc R U . . .
C10 C 0.2712(4) 0.4654(3) 0.87193(17) 0.0277(5) Uani 1 1 d . . . . .
H10 H 0.363103 0.462182 0.924912 0.033 Uiso 1 1 calc R U . . .
C11 C 0.0479(4) 0.3707(3) 0.89802(17) 0.0282(5) Uani 1 1 d . . . . .
H11 H -0.013165 0.302407 0.968684 0.034 Uiso 1 1 calc R U . . .
C12 C -0.0859(4) 0.3760(3) 0.82084(18) 0.0267(5) Uani 1 1 d . . . . .
H12 H -0.239340 0.311407 0.838753 0.032 Uiso 1 1 calc R U . . .
C13 C 0.0024(4) 0.4749(3) 0.71743(17) 0.0247(5) Uani 1 1 d . . . . .
H13 H -0.090914 0.478149 0.664944 0.030 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'
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
C2 N1 N2 110.64(17) . . ?
C2 N1 C5 129.70(19) . . ?
N2 N1 C5 119.65(17) . . ?
N3 N2 N1 106.89(18) . . ?
N2 N3 C1 109.55(19) . . ?
C7 N4 C3 116.49(19) . . ?
N3 C1 C2 108.01(18) . . ?
N3 C1 C8 121.9(2) . . ?
C2 C1 C8 130.1(2) . . ?
N1 C2 C1 104.91(17) . . ?
N1 C2 H2 127.5 . . ?
C1 C2 H2 127.5 . . ?
N4 C3 C4 123.9(2) . . ?
N4 C3 H3 118.1 . . ?
C4 C3 H3 118.1 . . ?
C5 C4 C3 117.7(2) . . ?
C5 C4 H4 121.1 . . ?
C3 C4 H4 121.1 . . ?
C4 C5 C6 120.1(2) . . ?
C4 C5 N1 119.6(2) . . ?
C6 C5 N1 120.2(2) . . ?
C5 C6 C7 117.5(2) . . ?
C5 C6 H6 121.2 . . ?
C7 C6 H6 121.2 . . ?
N4 C7 C6 124.3(2) . . ?
N4 C7 H7 117.9 . . ?
C6 C7 H7 117.9 . . ?
C13 C8 C9 118.9(2) . . ?
C13 C8 C1 121.3(2) . . ?
C9 C8 C1 119.8(2) . . ?
C10 C9 C8 120.4(2) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 120.3(2) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C12 C11 C10 119.8(2) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 120.4(2) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C12 C13 C8 120.2(2) . . ?
C12 C13 H13 119.9 . . ?
C8 C13 H13 119.9 . . ?
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
N1 C2 1.355(3) . ?
N1 N2 1.357(3) . ?
N1 C5 1.430(3) . ?
N2 N3 1.311(3) . ?
N3 C1 1.366(3) . ?
N4 C7 1.340(3) . ?
N4 C3 1.343(3) . ?
C1 C2 1.372(3) . ?
C1 C8 1.460(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(3) . ?
C6 C7 1.386(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.395(3) . ?
C8 C9 1.399(3) . ?
C9 C10 1.384(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.387(3) . ?
C12 H12 0.9500 . ?
C13 H13 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 N1 N2 N3 0.1(2) . . . . ?
C5 N1 N2 N3 179.13(18) . . . . ?
N1 N2 N3 C1 0.0(2) . . . . ?
N2 N3 C1 C2 -0.1(2) . . . . ?
N2 N3 C1 C8 179.86(19) . . . . ?
N2 N1 C2 C1 -0.1(3) . . . . ?
C5 N1 C2 C1 -179.06(18) . . . . ?
N3 C1 C2 N1 0.1(2) . . . . ?
C8 C1 C2 N1 -179.81(19) . . . . ?
C7 N4 C3 C4 -0.5(3) . . . . ?
N4 C3 C4 C5 0.4(3) . . . . ?
C3 C4 C5 C6 0.2(3) . . . . ?
C3 C4 C5 N1 179.80(18) . . . . ?
C2 N1 C5 C4 -152.3(2) . . . . ?
N2 N1 C5 C4 28.9(3) . . . . ?
C2 N1 C5 C6 27.4(3) . . . . ?
N2 N1 C5 C6 -151.5(2) . . . . ?
C4 C5 C6 C7 -0.6(3) . . . . ?
N1 C5 C6 C7 179.78(18) . . . . ?
C3 N4 C7 C6 0.0(3) . . . . ?
C5 C6 C7 N4 0.5(3) . . . . ?
N3 C1 C8 C13 -158.9(2) . . . . ?
C2 C1 C8 C13 21.0(4) . . . . ?
N3 C1 C8 C9 21.5(3) . . . . ?
C2 C1 C8 C9 -158.6(2) . . . . ?
C13 C8 C9 C10 0.7(3) . . . . ?
C1 C8 C9 C10 -179.71(19) . . . . ?
C8 C9 C10 C11 -0.3(3) . . . . ?
C9 C10 C11 C12 -0.2(3) . . . . ?
C10 C11 C12 C13 0.2(3) . . . . ?
C11 C12 C13 C8 0.2(3) . . . . ?
C9 C8 C13 C12 -0.7(3) . . . . ?
C1 C8 C13 C12 179.75(19) . . . . ?
