4-Ethyl-6,6-ethylenedithio-2-(2-methoxyethyl)-7-methoxymethylene-2,3,4,5,6,7-hexahydro-1,5-methano-1<i>H</i>-azocino[4,3-<i>b</i>]indol-3-one
Hökelek, Tuncer; Uludağ, Nesimi; Patır, Süleyman; Acta Crystallographica Section E 62 (2006) o791–o793; doi:10.1107/S1600536806002601

data_2208200
_publ_section_title
4-Ethyl-6,6-ethylenedithio-2-(2-methoxyethyl)-7-methoxymethylene-2,3,4,5,6,7-hexahydro-1,5-methano-1<i>H</i>-azocino[4,3-<i>b</i>]indol-3-one
_journal_coeditor_code           WN6414
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o791
_journal_page_last               o793
_journal_paper_doi               10.1107/S1600536806002601
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C23 H30 N2 O3 S2'
_chemical_formula_moiety         'C23 H30 N2 O3 S2'
_chemical_formula_sum            'C23 H30 N2 O3 S2'
_chemical_formula_weight         446.64
_chemical_name_systematic
;
4-Ethyl-6,6-ethylenedithio-2-(2-methoxyethyl)-7-methoxymethylene-
2,3,4,5,6,7-hexahydro-1,5-methano-1H-azocino[4,3-b]indol-3-one
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.164(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.897(3)
_cell_length_b                   7.0394(14)
_cell_length_c                   21.195(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      34.6
_cell_measurement_theta_min      3.2
_cell_volume                     2211.9(7)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            4215
_diffrn_reflns_theta_full        71.13
_diffrn_reflns_theta_max         71.13
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.403
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0876P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1813
_reflns_number_gt                2322
_reflns_number_total             4119
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6414.cif
_cod_data_source_block           I
_cod_original_cell_volume        2211.8(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2208200
_cod_database_fobs_code          2208200