1-Ethyl-4,4,6,8-tetramethyl-2-tosyl-2,3,3a,4,6,7,8,9-octahydro-1<i>H</i>-pyrrolo[3,4-<i>c</i>]pyrano[6,5-<i>d</i>]pyrimidine-7,9-dione
Chinnakali, K.; Sudha, D.; Jayagopi, M.; Raghunathan, R.; Fun, Hoong-Kun; Acta Crystallographica Section E 63 (2007) o4434–o4435; doi:10.1107/S160053680705221X

data_2216162
_publ_section_title
1-Ethyl-4,4,6,8-tetramethyl-2-tosyl-2,3,3a,4,6,7,8,9-octahydro-1<i>H</i>-pyrrolo[3,4-<i>c</i>]pyrano[6,5-<i>d</i>]pyrimidine-7,9-dione
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4434
_journal_page_last               o4435
_journal_paper_doi               10.1107/S160053680705221X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C22 H29 N3 O5 S'
_chemical_formula_moiety         'C22 H29 N3 O5 S'
_chemical_formula_sum            'C22 H29 N3 O5 S'
_chemical_formula_weight         447.55
_chemical_name_systematic
;
1-Ethyl-4,4,6,8-tetramethyl-2-tosyl-2,3,3a,4,6,7,8,9-octahydro-1H-\
pyrrolo[3,4-<i>c</i>]pyrano[6,5-<i>d</i>]pyrimidine-7,9-dione
;
_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                71.576(2)
_cell_angle_beta                 88.034(2)
_cell_angle_gamma                68.674(2)
_cell_formula_units_Z            4
_cell_length_a                   11.6929(3)
_cell_length_b                   11.7844(3)
_cell_length_c                   17.9339(4)
_cell_measurement_reflns_used    5742
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      2.32
_cell_volume                     2174.87(10)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type
;
Bruker SMART APEX2 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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0710
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45861
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  0.9576
_exptl_absorpt_correction_T_min  0.9368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.533
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         11377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0718P)^2^+1.2173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1664
_reflns_number_gt                7677
_reflns_number_total             11377
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn2209.cif
_cod_data_source_block           I
_cod_database_code               2216162
_cod_database_fobs_code          2216162