Synthesis and structural characterisation of neutral pentacoordinate silicon(iv) complexes with a tridentate dianionic N,N,S chelate ligand.
Kobelt, Claudia; Burschka, Christian; Bertermann, Rüdiger; Fonseca Guerra, C.; Bickelhaupt, F. Matthias; Tacke, Reinhold; Dalton transactions (Cambridge, England : 2003) 41 (2012) 2148–2162; doi:10.1039/c1dt11306b

data_7017656
_publ_section_title
;
 Synthesis and structural characterisation of neutral pentacoordinate
 silicon(iv) complexes with a tridentate dianionic N,N,S chelate ligand.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2148
_journal_page_last               2162
_journal_paper_doi               10.1039/c1dt11306b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         '2(C19 H15 F3 N2 O3 S2 Si), C7 H8'
_chemical_formula_sum            'C22.5 H19 F3 N2 O3 S2 Si'
_chemical_formula_weight         514.61
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.48(3)
_cell_angle_beta                 73.49(3)
_cell_angle_gamma                74.68(3)
_cell_formula_units_Z            2
_cell_length_a                   9.972(2)
_cell_length_b                   11.273(2)
_cell_length_c                   11.806(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      6.85
_cell_volume                     1141.3(5)
_computing_cell_refinement       Stoe-IPDS
_computing_data_collection       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_computing_molecular_graphics    OrteP/Povray
_computing_publication_material  Bruker-SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  Stoe_image_plate
_diffrn_measurement_method       omega_scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16511
_diffrn_reflns_theta_full        29.15
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.339
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       long_prism
_exptl_crystal_F_000             530
_exptl_crystal_size_max          .48
_exptl_crystal_size_mid          .32
_exptl_crystal_size_min          .15
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5598
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.2554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                4307
_reflns_number_total             5598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11306b.txt
_cod_data_source_block           kob12cu_6
_cod_original_cell_volume        1141.3(4)
_cod_original_formula_sum        'C22.50 H19 F3 N2 O3 S2 Si'
_cod_database_code               7017656