Methyl 4-(4-chlorophenyl)-3,3a,4,4a,5,12c-hexahydro-2-thianaphtho[1',2':3,2]furo[5,4-<i>b</i>]pyrrolizine-4a-carboxylate
Selvanayagam, S.; Sridhar, B.; Ravikumar, K.; Kathiravan, S.; Raghunathan, R.; Acta Crystallographica Section E 66 (2010) o2098–; doi:10.1107/S1600536810028746

data_2227020
_publ_section_title
;
 Methyl
 4-(4-chlorophenyl)-3,3a,4,4a,5,12c-hexahydro-2-thianaphtho[1',2':3,2]furo[5,4-<i>b</i>]pyrrolizine-4a-carboxylate
;
_journal_coeditor_code           NG5001
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2098
_journal_paper_doi               10.1107/S1600536810028746
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C25 H22 Cl N O3 S'
_chemical_formula_moiety         'C25 H22 Cl N O3 S'
_chemical_formula_sum            'C25 H22 Cl N O3 S'
_chemical_formula_weight         451.95
_chemical_name_systematic
;
Methyl 4-(4-chlorophenyl)-3,3a,4,4a,5,12c-hexahydro-2-
thianaphtho[1',2':3,2]furo[5,4-<i>b</i>]pyrrolizine-4a-carboxylate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0740(6)
_cell_length_b                   12.1109(8)
_cell_length_c                   22.1813(15)
_cell_measurement_reflns_used    16148
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.1
_cell_volume                     2169.0(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
;
ORTEP3 (Farrugia, 1997) and PLATON (Spek, 2009)
;
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25236
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         1.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.148
_refine_ls_abs_structure_details 'Flack (1983), 2186 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0624P)^2^+0.2403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                4559
_reflns_number_total             5157
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng5001.cif
_cod_data_source_block           I
_cod_database_code               2227020
_cod_database_fobs_code          2227020