Methyl 2-methyl-5-oxo-4-(2-thienyl)-1,5,7,8,9,10-hexahydro-4<i>H</i>-pyrido[2',3':3,4]pyrrolo[1,2-<i>a</i>][1,3]diazepine-3-carboxylate
Vrábel, Viktor; Kožíšek, Jozef; Marchalín, Štefan; Svoboda, Ingrid; Acta Crystallographica Section E 61 (2005) o733–o735; doi:10.1107/S1600536805005209

data_2205280
_publ_section_title
;Methyl
 2-methyl-5-oxo-4-(2-thienyl)-1,5,7,8,9,10-hexahydro-4<i>H</i>-pyrido[2',3':3,4]pyrrolo[1,2-<i>a</i>][1,3]diazepine-3-carboxylate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o733
_journal_page_last               o735
_journal_paper_doi               10.1107/S1600536805005209
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C18 H19 N3 O3 S'
_chemical_formula_moiety         'C18 H19 N3 O3 S'
_chemical_formula_sum            'C18 H19 N3 O3 S'
_chemical_formula_weight         357.42
_chemical_name_systematic
;
Methyl 2-methyl-5-oxo-4-(2-thienyl)-1,5,7,8,9,10-hexahydro-4H-
pyrido[2',3':3,4]pyrrolo[1,2-a][1,3]diazepine-3-carboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.94(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.050(3)
_cell_length_b                   16.492(5)
_cell_length_c                   10.737(5)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      44.92
_cell_measurement_theta_min      40.14
_cell_volume                     1741.1(11)
_computing_cell_refinement       'STADI4 and DIF4'
_computing_data_collection
'STADI4 (Stoe & Cie, 1991) and DIF4 (Stoe & Cie, 1991)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1993)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe Stadi-4'
_diffrn_measurement_method       'profile data from \q/2\q'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.00000
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3440
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.9213
_exptl_absorpt_correction_T_min  0.8852
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.369
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0977P)^2^+0.9592P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1670
_refine_ls_wR_factor_ref         0.1905
_reflns_number_gt                2379
_reflns_number_total             3436
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            hg6144.cif
_cod_data_source_block           I
_cod_original_cell_volume        1741.2(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2205280
_cod_database_fobs_code          2205280