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_4106488
_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 H30 N2 O4 S Si3'
_chemical_formula_weight         466.78
_chemical_name_systematic
; 
 (2,4-dinitrophenyl)thiotetrahedrane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 117.6900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.2544(19)
_cell_length_b                   13.9007(13)
_cell_length_c                   20.932(2)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.27
_cell_volume                     5218.5(9)
_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      120
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28354
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  0.9449
_exptl_absorpt_correction_T_min  0.9064
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       plate
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         11598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+15.7440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1613
_reflns_number_gt                9937
_reflns_number_total             11598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205361a_si_002.cif
_cod_data_source_block           dinitro2_0m
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4106488