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
Riedel, Sophie; Gerwig, Maik; Gerlach, Daniela; Brendler, Erica; Gericke, Robert; Kroke, Edwin; Wagler, Jörg; Inorganics 11 (2023) 473–; doi:10.3390/inorganics11120473

data_1570716
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0780P)^2^+0.0403P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              35070
_shelx_hkl_checksum              96627