Crystal structure of methyl 7-phenyl-6a,7,7a,8,9,10-hexahydro-6<i>H</i>,11a<i>H</i>-thiochromeno[3,4-<i>b</i>]pyrrolizine-6a-carboxylate
Savithri, M. P.; Suresh, M.; Raghunathan, R.; Raja, R.; SubbiahPandi, A.; Acta Crystallographica Section E 71 (2015) o627–o628; doi:10.1107/S2056989015014024

data_2240980
_publ_section_title
;
 Crystal structure of methyl
 7-phenyl-6a,7,7a,8,9,10-hexahydro-6<i>H</i>,11a<i>H</i>-thiochromeno[3,4-<i>b</i>]pyrrolizine-6a-carboxylate
;
_journal_coeditor_code           SU5170
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o627
_journal_page_last               o628
_journal_paper_doi               10.1107/S2056989015014024
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C22 H23 N O2 S'
_chemical_formula_moiety         'C22 H23 N O2 S'
_chemical_formula_sum            'C22 H23 N O2 S'
_chemical_formula_weight         365.47
_chemical_name_systematic
'Methyl 7-phenyl-6a,7,7a,8,9,10-hexahydro-6<i>H</i>,11a<i>H</i>-thiochromeno[3,4-<i>b</i>]pyrrolizine-6a-carboxylate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                81.270(2)
_cell_angle_beta                 66.626(2)
_cell_angle_gamma                74.385(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5184(4)
_cell_length_b                   10.4041(5)
_cell_length_c                   10.6923(4)
_cell_measurement_reflns_used    3265
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.08
_cell_volume                     934.88(7)
_computing_cell_refinement
;
SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2004)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_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      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f 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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18019
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  0.9542
_exptl_absorpt_correction_T_min  0.9454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.209
_refine_ls_extinction_coef       0.025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3265
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0453P)^2^+0.4695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                2504
_reflns_number_total             3265
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su5170sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-P  1'
_cod_database_code               2240980
_cod_database_fobs_code          2240980