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_4108295
_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_absolute_configuration unk
_chemical_formula_sum            'C20 H38 I N O Si Sn'
_chemical_formula_weight         582.19
_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   geom
_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                   8.9491(9)
_cell_length_b                   14.9054(14)
_cell_length_c                   18.5409(18)
_cell_measurement_reflns_used    8598
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.397
_cell_measurement_theta_min      2.527
_cell_volume                     2473.2(4)
_computing_cell_refinement       'SAINT V7.34A'
_computing_data_collection       'APEX2 v2.1-4'
_computing_data_reduction        'SAINT V7.34A'
_computing_molecular_graphics
;
 XP in SHELXTL ver. 6.10 and ORTEP-3, Farrugia
;
_computing_publication_material
;
 XP in SHELXTL ver. 6.10 and ORTEP-3, Farrugia
;
_computing_structure_refinement  'SHELXL in SHELXTL ver. 6.10'
_computing_structure_solution    'SHELXS in SHELXTL ver. 6.10'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-CCD'
_diffrn_measurement_method       'omega scans'
_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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            39343
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    2.338
_exptl_absorpt_correction_T_max  0.7998
_exptl_absorpt_correction_T_min  0.4548
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2007/5
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0242P)^2^+2.3631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                4430
_reflns_number_total             4563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja711104q-file002.cif
_cod_data_source_block           tin
_cod_database_code               4108295