(4<i>S</i>,5<i>S</i>)-4,5-Bis(3-cyclohexyl-2-thioxobenzimidazol-1-ylmethyl)-2,2-dimethyl-1,3-dioxolane from synchrotron data
Marshall, Colin; Harrison, William T. A.; Acta Crystallographica Section E 63 (2007) o4502–o4502; doi:10.1107/S1600536807053342

data_2216765
_publ_section_title
;(4<i>S</i>,5<i>S</i>)-4,5-Bis(3-cyclohexyl-2-thioxobenzimidazol-1-ylmethyl)-2,2-dimethyl-1,3-dioxolane
 from synchrotron data
;
_journal_coeditor_code           SJ2390
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4502
_journal_page_last               o4502
_journal_paper_doi               10.1107/S1600536807053342
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C33 H42 N4 O2 S2'
_chemical_formula_moiety         'C33 H42 N4 O2 S2'
_chemical_formula_sum            'C33 H42 N4 O2 S2'
_chemical_formula_weight         590.83
_chemical_name_systematic
;
(4S,5S)-4,5-Bis(3-cyclohexyl-2-thioxobenzimidazol-1-ylmethyl)-2,2-dimethyl-\
1,3-dioxolane
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 95.398(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.876(6)
_cell_length_b                   10.652(3)
_cell_length_c                   14.120(4)
_cell_measurement_reflns_used    3328
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.18
_cell_volume                     3275.7(16)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Daresbury synchrotron'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68710
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0808
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11222
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.403
_refine_ls_abs_structure_details 'Flack (1983), 3144 Friedel pairs'
_refine_ls_abs_structure_Flack   0.07(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7522
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0671P)^2^+0.1687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                5903
_reflns_number_total             7522
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2390.cif
_cod_data_source_block           I
_cod_original_cell_volume        3275.5(16)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2216765
_cod_database_fobs_code          2216765