Influence of the Silyl Group on the Reactivity of Some Ortho-Lithiated Aryl Alkyl Sulfides
Durka, Krzysztof; Kliś, Tomasz; Serwatowski, Janusz; Woźniak, Krzysztof; Organometallics 32 (2013) 3145–; doi:10.1021/om400236x

data_4089467
_publ_section_title
;
 Influence of the Silyl Group on the Reactivity of Some Ortho-Lithiated
 Aryl Alkyl Sulfides
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3145
_journal_paper_doi               10.1021/om400236x
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C16 H18 S Si'
_chemical_formula_sum            'C16 H18 S Si'
_chemical_formula_weight         270.45
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 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            8
_cell_length_a                   15.5250(5)
_cell_length_b                   8.2613(3)
_cell_length_c                   22.6528(7)
_cell_measurement_reflns_used    5171
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2145
_cell_measurement_theta_min      1.7943
_cell_volume                     2905.37(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.1 (release 27-01-2011 CrysAlis171 .NET)
(compiled Feb 15 2011,21:22:45)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.1 (release 27-01-2011 CrysAlis171 .NET)
(compiled Feb 15 2011,21:22:45)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.1 (release 27-01-2011 CrysAlis171 .NET)
(compiled Feb 15 2011,21:22:45)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'KUMA CCD'
_diffrn_measurement_method       'omega scan'
_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  0.0723
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            24723
_diffrn_reflns_theta_full        32.29
_diffrn_reflns_theta_max         32.29
_diffrn_reflns_theta_min         1.80
_diffrn_standards_interval_count '5o frames'
_diffrn_standards_number         '1 frame'
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         9163
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0568P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                6085
_reflns_number_total             9163
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400236x_si_001.cif
_cod_data_source_block           11
_cod_original_sg_symbol_Hall     P2c-2n
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               4089467