Crystal structures of methyl 3-(4-isopropylphenyl)-1-methyl-1,2,3,3a,4,9b-hexahydrothiochromeno[4,3-<i>b</i>]pyrrole-3a-carboxylate, methyl 1-methyl-3-(<i>o</i>-tolyl)-1,2,3,3a,4,9b-hexahydrothiochromeno[4,3-<i>b</i>]pyrrole-3a-carboxylate and methyl 1-methyl-3-(<i>o</i>-tolyl)-3,3a,4,9b-tetrahydro-1<i>H</i>-thiochromeno[4,3-<i>c</i>]isoxazole-3a-carboxylate
Raja, R.; Suresh, M.; Raghunathan, R.; SubbiahPandi, A.; Acta Crystallographica Section E 71 (2015) 574–577; doi:10.1107/S2056989015008063

data_2240601
_publ_section_title
;
 Crystal structures of methyl
 3-(4-isopropylphenyl)-1-methyl-1,2,3,3a,4,9b-hexahydrothiochromeno[4,3-<i>b</i>]pyrrole-3a-carboxylate,
 methyl
 1-methyl-3-(<i>o</i>-tolyl)-1,2,3,3a,4,9b-hexahydrothiochromeno[4,3-<i>b</i>]pyrrole-3a-carboxylate
 and methyl
 1-methyl-3-(<i>o</i>-tolyl)-3,3a,4,9b-tetrahydro-1<i>H</i>-thiochromeno[4,3-<i>c</i>]isoxazole-3a-carboxylate
;
_journal_coeditor_code           SU5106
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              574
_journal_page_last               577
_journal_paper_doi               10.1107/S2056989015008063
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C21 H21 N O2 S'
_chemical_formula_moiety         'C21 H21 N O2 S'
_chemical_formula_sum            'C21 H21 N O2 S'
_chemical_formula_weight         351.45
_chemical_name_systematic
'Methyl 1-methyl-3-(<i>o</i>-tolyl)-1,2,3,3a,4,9b-hexahydrothiochromeno[4,3-<i>b</i>]pyrrole-3a-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           SHELXL97
_cell_angle_alpha                104.5540(10)
_cell_angle_beta                 90.9830(10)
_cell_angle_gamma                90.1340(10)
_cell_formula_units_Z            2
_cell_length_a                   8.1882(3)
_cell_length_b                   10.4987(4)
_cell_length_c                   10.9594(4)
_cell_measurement_reflns_used    2790
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.92
_cell_volume                     911.74(6)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2008)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2008)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2008)
;
_computing_molecular_graphics
;
<i>ORTEP-3</i> for Windows (Farrugia, 2012)
;
_computing_publication_material
;
<i>SHELXL97</i> (Sheldrick, 2008) and <i>PLATON</i> (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19010
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.92
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0591P)^2^+0.2766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                2790
_reflns_number_total             3210
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su5106sup1.cif
_cod_data_source_block           II
_cod_database_code               2240601
_cod_database_fobs_code 2240601