Structure/Reactivity Studies on an α-Lithiated Benzylsilane: Chemical Interpretation of Experimental Charge Density
Holger Ott; Christian Däschlein; Dirk Leusser; Daniel Schildbach; Timo Seibel; Dietmar Stalke; Carsten Strohmann; Journal of the American Chemical Society 130 (2008) 11901–11911; doi:10.1021/ja711104q

data_4108294
_publ_contact_author             'Prof. Dr. D. Stalke'
_publ_contact_author_email       dstalke@chemie.uni-goettingen.de
_publ_section_title
;
 Structure/Reactivity Studies on an \a-Lithiated Benzylsilane: Chemical
 Interpretation of Experimental Charge Density
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11901
_journal_page_last               11911
_journal_paper_doi               10.1021/ja711104q
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C23 H39 Li N2 O Si'
_chemical_formula_weight         394.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5424(7)
_cell_length_b                   11.2137(8)
_cell_length_c                   21.7553(16)
_cell_measurement_reflns_used    9475
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.384
_cell_measurement_theta_min      2.330
_cell_volume                     2327.9(3)
_computing_cell_refinement       'SAINT V7.23A'
_computing_data_collection       'APEX2 v2.0-2'
_computing_data_reduction        'SAINT V7.23A'
_computing_molecular_graphics
;
XP in SHELXTL ver. 6.10 and XDGRAPH in XD2006,
Volkov et al., and ORTEP-3, Farrugia
;
_computing_publication_material
;
XP in SHELXTL ver. 6.10 and XD2006,
Volkov et al. and ORTEP-3, Farrugia
;
_computing_structure_refinement
;
IAM with SHELXL in SHELXTL ver. 6.10; multipole refinement 
with XDLSM in  XD2006, Volkov et al.
;
_computing_structure_solution    'SHELXS in SHELXTL ver. 6.10'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device_type  'Bruker TXS with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayer Mo mirrors'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0103
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            24516
_diffrn_reflns_theta_max         50.09
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2006/3
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.134
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.595
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         21027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.595
_refine_ls_R_factor_all          0.029
_refine_ls_R_factor_gt           0.02
_refine_ls_R_Fsqd_factor         0.024
_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 w2 = 1/[s^2^(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.031
_reflns_number_gt                22015
_reflns_number_total             24516
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            ja711104q-file001.cif
_cod_data_source_block           stroh1b
_cod_database_code               4108294