<i>cis</i>-4,4,10-Trimethyl-2-tosyl-1,2,3,3a,4,11b-hexahydro-11<i>H</i>-pyrrolo[3,4-<i>c</i>]pyrano[5,6-<i>c</i>]quinolin-11-one hemihydrate
K. Chinnakali; D. Sudha; M. Jayagopi; R. Raghunathan; Hoong-Kun Fun; Acta Crystallographica Section E 63 (2007) o4489–o4490; doi:10.1107/S1600536807053287

data_2216165
_publ_section_title
;<i>cis</i>-4,4,10-Trimethyl-2-tosyl-1,2,3,3a,4,11b-hexahydro-11<i>H</i>-pyrrolo[3,4-<i>c</i>]pyrano[5,6-<i>c</i>]quinolin-11-one
 hemihydrate
;
_journal_coeditor_code           WN2212
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4489
_journal_page_last               o4490
_journal_paper_doi               10.1107/S1600536807053287
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C24 H26 N2 O4 S, 0.5H2 O'
_chemical_formula_moiety         'C24 H26 N2 O4 S, 0.5(H2 O)'
_chemical_formula_sum            'C24 H27 N2 O4.5 S'
_chemical_formula_weight         447.54
_chemical_name_systematic
;
cis-4,4,10-Trimethyl-2-tosyl-1,2,3,3a,4,11b-hexahydro-
11H-pyrrolo[3,4-<i>c</i>]pyrano[5,6-<i>c</i>]quinolin-11-one hemihydrate
;
_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                 111.3360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.1413(3)
_cell_length_b                   14.7008(3)
_cell_length_c                   20.9973(4)
_cell_measurement_reflns_used    6683
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.81
_cell_measurement_theta_min      2.49
_cell_volume                     4353.45(15)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1998)'
_computing_publication_material
;
SHELXTL (Sheldrick, 1998) and PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 1998)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Bruker SMART APEXII CCD area-detector
;
_diffrn_measurement_method       \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  0.0834
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            127879
_diffrn_reflns_theta_full        30.15
_diffrn_reflns_theta_max         30.15
_diffrn_reflns_theta_min         1.44
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.9879
_exptl_absorpt_correction_T_min  0.9138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.484
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         12850
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0482P)^2^+1.9763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1292
_reflns_number_gt                9240
_reflns_number_total             12850
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn2212.cif
_cod_data_source_block           I
_cod_original_cell_volume        4353.44(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C24 H27 N2 O4.50 S'
_cod_database_code               2216165
_cod_database_fobs_code          2216165