Bis[3α,7α,12α-tris(4-nitrobenzoyloxy)-5β-cholan-24-yl] disulfide–ethyl acetate–<i>n</i>-hexane (4/4/1)
Brzezinski, Krzysztof; Tomkiel, Aneta M.; Łotowski, Zenon; Morzycki, Jacek; Dauter, Zbigniew; Acta Crystallographica Section E 67 (2011) o74–o75; doi:10.1107/S1600536810050385

data_2228715
_publ_section_title
;
 Bis[3\a,7\a,12\a-tris(4-nitrobenzoyloxy)-5\b-cholan-24-yl]
 disulfide--ethyl acetate--<i>n</i>-hexane (4/4/1)
;
_journal_coeditor_code           GK2316
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o74
_journal_page_last               o75
_journal_paper_doi               10.1107/S1600536810050385
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C90 H100 N6 O24 S2, C4 H8 O2, 0.25C6 H14'
_chemical_formula_moiety         'C90 H100 N6 O24 S2, C4 H8 O2, 0.25(C6 H14)'
_chemical_formula_sum            'C95.5 H111.5 N6 O26 S2'
_chemical_formula_weight         1823.53
_chemical_name_systematic
;
Bis[3\a,7\a,12\a-tris(4-nitrobenzoyloxy)-5\b-cholan-24-yl] disulfide--ethyl
acetate--<i>n</i>-hexane (4/4/1)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.81(2)
_cell_length_b                   26.47(3)
_cell_length_c                   30.77(3)
_cell_measurement_reflns_used    88841
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      0.98
_cell_volume                     18578(3)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'NECAT APS beamline Software'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and PyMOL (DeLano, 2002)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Mar MAR315 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Si111 double crystal'
_diffrn_radiation_source         'NECAT 24ID-C synchrotron beamline APS, USA'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.59040
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            247079
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         0.98
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski <i>et al.</i>, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             7732
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.775
_refine_diff_density_min         -0.814
_refine_ls_abs_structure_details 'Flack (1983), 39133 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2324
_refine_ls_number_reflns         88841
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+2.7163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                85229
_reflns_number_total             88841
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gk2316.cif
_cod_data_source_block           I
_cod_original_cell_volume        1858E1(3)
_cod_database_code               2228715
_cod_database_fobs_code          2228715