Si-E (E = N, O, F) Bonding in a Hexacoordinated Silicon Complex: New Facts from Experimental and Theoretical Charge Density Studies
Nikolaus Kocher; Julian Henn; Boris Gostevskii; Daniel Kost; Inna Kalikhman; Bernd Engels; Dietmar Stalke; Journal of the American Chemical Society 126 (2004) 5563–5568; doi:10.1021/ja038459r

data_4112529
_publ_contact_author             'Prof. Dr. D. Stalke'
_publ_contact_author_email       dstalke@chemie.uni-wuerzburg.de
_publ_section_title
;
 Si-E (E = N, O, F) Bonding in a Hexacoordinated Silicon Complex: New
 Facts from Experimental and Theoretical Charge Density Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5563
_journal_page_last               5568
_journal_paper_doi               10.1021/ja038459r
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C18 H22 F2 N4 O2 Si'
_chemical_formula_weight         392.49
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 113.7310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8444(7)
_cell_length_b                   8.5365(3)
_cell_length_c                   12.0682(4)
_cell_measurement_reflns_used    7151
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.242
_cell_volume                     1871.51(11)
_computing_cell_refinement       'SAINT-NT V5/6.28A'
_computing_data_collection       'SMART-NT V5.624'
_computing_data_reduction        'SAINT-NT V5/6.28A'
_computing_molecular_graphics    'SHELXTL-NT V5.1'
_computing_publication_material  'SHELXTL-NT V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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
'0.0537 (low angle batch), 0.0738 (high angle batch)'
_diffrn_reflns_av_sigmaI/netI
'0.0084 (low angle batch), 0.0303 (high angle batch)'
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number
'24118 (low angle batch), 29791 (high angle batch)'
_diffrn_reflns_theta_full        54.34
_diffrn_reflns_theta_max         54.34
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  1.184
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         11448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0749P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1052
_reflns_number_gt                9506
_reflns_number_total             11448
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja038459rsi20030911_042051.cif
_cod_data_source_block           1
_cod_database_code               4112529