3-Benzyl-7-methyl-9-phenyl-2-tosyl-2,3,3a,4,9,9a-hexahydro-1<i>H</i>-pyrrolo[3,4-<i>b</i>]quinoline
Chinnakali, K.; Sudha, D.; Jayagobi, M.; Raghunathan, R.; Fun, Hoong-Kun; Acta Crystallographica Section E 65 (2009) o2924–o2925; doi:10.1107/S1600536809044481

data_2224044
_publ_section_title
3-Benzyl-7-methyl-9-phenyl-2-tosyl-2,3,3a,4,9,9a-hexahydro-1<i>H</i>-pyrrolo[3,4-<i>b</i>]quinoline
_journal_coeditor_code           TK2561
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2924
_journal_page_last               o2925
_journal_paper_doi               10.1107/S1600536809044481
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C32 H32 N2 O2 S'
_chemical_formula_moiety         'C32 H32 N2 O2 S'
_chemical_formula_sum            'C32 H32 N2 O2 S'
_chemical_formula_weight         508.66
_chemical_name_systematic
;
3-Benzyl-7-methyl-9-phenyl-2-tosyl-2,3,3a,4,9,9a-hexahydro-1<i>H</i>-
pyrrolo[3,4-<i>b</i>]quinoline
;
_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                 96.294(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0445(4)
_cell_length_b                   10.6014(4)
_cell_length_c                   27.5330(10)
_cell_measurement_reflns_used    5605
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.09
_cell_measurement_theta_min      2.27
_cell_volume                     2624.07(18)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0784
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            22823
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.9736
_exptl_absorpt_correction_T_min  0.3601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.505
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0606
_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^)+(0.1011P)^2^+1.1335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1784
_reflns_number_gt                3615
_reflns_number_total             5138
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2561.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2224044
_cod_database_fobs_code          2224044