Sulfur-Substituted Tetrahedranes
Tatsumi Ochiai; Masaaki Nakamoto; Yusuke Inagaki; Akira Sekiguchi; Journal of the American Chemical Society 133 (2011) 11504–11507; doi:10.1021/ja205361a

data_4106487
_publ_section_title
;
 Sulfur-Substituted Tetrahedranes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11504
_journal_page_last               11507
_journal_paper_doi               10.1021/ja205361a
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C19 H31 N O2 S Si3'
_chemical_formula_weight         421.78
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.9630(10)
_cell_angle_beta                 95.4370(10)
_cell_angle_gamma                99.0200(10)
_cell_formula_units_Z            4
_cell_length_a                   9.3927(5)
_cell_length_b                   17.0136(9)
_cell_length_c                   17.3220(9)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.34
_cell_volume                     2499.7(2)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27789
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  0.9477
_exptl_absorpt_correction_T_min  0.8968
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         11075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.7769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                9204
_reflns_number_total             11075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205361a_si_001.cif
_cod_data_source_block           tdsc6h4no2_0m
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4106487