Neutral Pentacoordinate Silicon Fluorides Derived from Amidinate, Guanidinate, and Triazapentadienate Ligands and Base-Induced Disproportionation of Si2Cl6 to Stable Silylenes
Rajendra S. Ghadwal; Kevin Pröpper; Birger Dittrich; Peter G. Jones; Herbert W. Roesky; Inorganic Chemistry 50 (2011) 358–364; doi:10.1021/ic1020548

data_4324171
_publ_contact_author_address
;
Institut f\"ur Anorganische Chemie
Georg-August-Universit\"at G\"ottingen 
Tammanstr. 4, 37077 G\"ottingen (Germany)
;
_publ_contact_author_email       hroesky@gwdg.de
_publ_contact_author_name        'Herbert W. Roesky'
_publ_section_title
;
 Neutral Pentacoordinate Silicon Fluorides Derived from Amidinate,
 Guanidinate, and Triazapentadienate Ligands and Base-Induced
 Disproportionation of Si2Cl6 to Stable Silylenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              358
_journal_page_last               364
_journal_paper_doi               10.1021/ic1020548
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C15 H23 F3 N2 Si'
_chemical_formula_weight         316.44
_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                93.738(9)
_cell_angle_beta                 100.701(9)
_cell_angle_gamma                107.182(9)
_cell_formula_units_Z            2
_cell_length_a                   8.7620(9)
_cell_length_b                   8.9751(9)
_cell_length_c                   10.9816(12)
_cell_measurement_reflns_used    12630
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3761
_cell_measurement_theta_min      2.7823
_cell_volume                     804.05(16)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_collection
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1057
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23331
_diffrn_reflns_theta_full        30.99
_diffrn_reflns_theta_max         30.99
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         5091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                4097
_reflns_number_total             5091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1020548_si_003.cif
_cod_data_source_block           rs01goe
_cod_original_cell_volume        804.05(15)
_cod_database_code               4324171