Crystal structure of (±)-(3a<i>R</i>,5<i>R</i>,8b<i>R</i>)-5-hydroperoxy-2-phenyl-6-tosyl-4,5,6,8b-tetrahydropyrrolo[3,4-<i>e</i>]indole-1,3(2<i>H</i>,3a<i>H</i>)-dione
Noland, Wayland E.; Gullickson, Glen C.; Dickson, Rozalin R.; Groess, Leah L.; Tritch, Kenneth J.; Acta Crystallographica Section E 70 (2014) 192–195; doi:10.1107/S1600536814019874

data_2239993
_publ_section_title
;
 Crystal structure of
 (+-)-(3a<i>R</i>,5<i>R</i>,8b<i>R</i>)-5-hydroperoxy-2-phenyl-6-tosyl-4,5,6,8b-tetrahydropyrrolo[3,4-<i>e</i>]indole-1,3(2<i>H</i>,3a<i>H</i>)-dione
;
_journal_coeditor_code           HB7256
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              192
_journal_page_last               195
_journal_paper_doi               10.1107/S1600536814019874
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C23 H20 N2 O6 S'
_chemical_formula_moiety         'C23 H20 N2 O6 S'
_chemical_formula_sum            'C23 H20 N2 O6 S'
_chemical_formula_weight         452.48
_chemical_melting_point          425
_chemical_name_systematic
(+-)-(3a<i>R</i>,5<i>R</i>,8b<i>R</i>)-5-Hydroperoxy-2-phenyl-6-tosyl-4,5,6,8b-tetrahydropyrrolo[3,4-<i>e</i>]indole-1,3(2<i>H</i>,3a<i>H</i>)-dione
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                102.068(3)
_cell_angle_beta                 107.786(2)
_cell_angle_gamma                96.364(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6563(13)
_cell_length_b                   9.8819(15)
_cell_length_c                   13.533(2)
_cell_measurement_reflns_used    2698
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.49
_cell_volume                     1058.8(3)
_computing_cell_refinement
;
SAINT (Bruker, 2003)
;
_computing_data_collection
;
SMART (Bruker, 2001)
;
_computing_data_reduction
;
SAINT (Bruker, 2003)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), enCIFer (Allen <i>et al.</i>,
2004), and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10544
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.9617
_exptl_absorpt_correction_T_min  0.8909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3751
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.2551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                3194
_reflns_number_total             3751
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7256sup1.cif
_cod_data_source_block           I
_cod_database_code               2239993
_cod_database_fobs_code          2239993