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_1570713
_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+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.277
_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/[\s^2^(Fo^2^)+(0.0207P)^2^+0.7118P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_estimated_absorpt_t_min   0.709
_shelx_estimated_absorpt_t_max   0.850
_shelx_res_checksum              48220
_shelx_hkl_checksum              88952