Crystal structure of ethyl (2<i>S</i>)-9-methoxy-2-methyl-4-oxo-3,4,5,6-tetrahydro-2<i>H</i>- 2,6-methanobenzo[<i>g</i>][1,3,5]oxadiazocine-11-carboxylate
Dhandapani, A.; Manivarman, S.; Subashchandrabose, S.; Gunasekaran, B.; Acta Crystallographica Section E 71 (2015) o117–o118; doi:10.1107/S2056989015000559

data_2240397
_publ_section_title
;
 Crystal structure of ethyl
 (2<i>S</i>)-9-methoxy-2-methyl-4-oxo-3,4,5,6-tetrahydro-2<i>H</i>-
 2,6-methanobenzo[<i>g</i>][1,3,5]oxadiazocine-11-carboxylate
;
_journal_coeditor_code           SU5057
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o117
_journal_page_last               o118
_journal_paper_doi               10.1107/S2056989015000559
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C15 H18 N2 O5'
_chemical_formula_moiety         'C15 H18 N2 O5'
_chemical_formula_sum            'C15 H18 N2 O5'
_chemical_formula_weight         306.31
_chemical_name_common
'Ethyl 5-methoxy-9-methyl-11-oxo-8-oxa-10,12-diazatricyclo[7.3.1.0^2,7^]trideca-2(7),3,5-triene-13-carboxylate'
_chemical_name_systematic
;Ethyl (2<i>S</i>)-9-methoxy-2-methyl-4-oxo-3,4,5,6-tetrahydro-2<i>H</i>-
2,6-methanobenzo[<i>g</i>][1,3,5]oxadiazocine-11-carboxylate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.252(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6982(14)
_cell_length_b                   7.4802(12)
_cell_length_c                   10.8293(17)
_cell_measurement_reflns_used    3030
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.8
_cell_measurement_theta_min      2.0
_cell_volume                     732.2(2)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008, 2015)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w and \f'
_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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10886
_diffrn_reflns_theta_full        26.89
_diffrn_reflns_theta_max         26.89
_diffrn_reflns_theta_min         2.02
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.9750
_exptl_absorpt_correction_T_min  0.9540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.248
_refine_ls_abs_structure_details
;
Flack (1983),  1371 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       0.031(8)
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3030
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0713
_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^)+(0.0537P)^2^+0.7506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1749
_reflns_number_gt                2029
_reflns_number_total             3030
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su5057sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2240397
_cod_database_fobs_code          2240397