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
Seidel, Anne; Weigel, Mareike; Ehrlich, Lisa; Gericke, Robert; Brendler, Erica; Wagler, Jörg; Crystals 12 (2022) 1054–; doi:10.3390/cryst12081054

data_1567434
_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         'C22 H18 N2 O2 Si'
_chemical_formula_sum            'C22 H18 N2 O2 Si'
_chemical_formula_weight         370.47
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                88.692(3)
_cell_angle_beta                 88.561(3)
_cell_angle_gamma                81.453(3)
_cell_formula_units_Z            3
_cell_length_a                   6.1626(2)
_cell_length_b                   8.8822(3)
_cell_length_c                   26.4639(9)
_cell_measurement_reflns_used    65483
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.76
_cell_volume                     1431.76(8)
_computing_molecular_graphics    ShelXT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0197
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            48444
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.759
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.9450
_exptl_absorpt_correction_T_min  0.9231
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XShape
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       piece
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 5458 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         13251
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0536P)^2^+0.3504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    0.929
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                12147
_reflns_number_total             13251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file
CIFs_all-in-one_SeidelWeigelEhrlichGerickeBrendlerWagler_pyOpyS-silanes.cif
_cod_data_source_block           as-002d_01
_cod_database_code               1567434
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              49987
_shelx_hkl_checksum              63093