Reversible Neutral Dissociation of the N–Si Dative Bond in Hexacoordinate Hydrido Complexes of Silicon
Kalikhman, Inna; Kertsnus-Banchik, Evgenia; Gostevskii, Boris; Kocher, Nikolaus; Stalke, Dietmar; Kost, Daniel; Organometallics 28 (2009) 512–516; doi:10.1021/om8008487

data_4063614
_publ_contact_author             'Prof. Dr. D. Stalke, Prof. D. Kost'
_publ_contact_author_email
'dstalke@chemie.uni-wuerzburg.de; kostd@bgu.ac.il'
_publ_section_title
;
 Reversible Neutral Dissociation of the N--Si Dative Bond in
 Hexacoordinate Hydrido Complexes of Silicon
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              512
_journal_page_last               516
_journal_paper_doi               10.1021/om8008487
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C14 H18 F6 N4 O2 Si'
_chemical_formula_weight         416.41
_chemical_name_common            10b
_chemical_name_systematic
; 
 [N-(dimethylamino)trifluoroacetimidato-N',O]hydridophenylsilicon(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.0130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9337(9)
_cell_length_b                   7.8090(5)
_cell_length_c                   17.1515(10)
_cell_measurement_reflns_used    5882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26371
_cell_measurement_theta_min      2.372
_cell_volume                     1812.57(19)
_computing_cell_refinement       'SAINT-NT V5/6.0'
_computing_data_collection       'SMART-NT V5.624'
_computing_data_reduction        'SAINT-NT V5/6.0'
_computing_molecular_graphics    'XP in SHELXL-97'
_computing_publication_material  'XP in SHELXL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex on D8-Goniometer'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19375
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.906347
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS2.05 (Sheldrick 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.9568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                3442
_reflns_number_total             3700
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            om8008487_si_001.cif
_cod_data_source_block           10b
_cod_original_sg_symbol_H-M      p2(1)/n
_cod_database_code               4063614