Crystal structure of 3-methoxycarbonyl-2-(4-methoxyphenyl)-8-oxo-1-azaspiro[4.5]deca-1,6,9-trien-1-ium-1-olate
Martins, Lucimara Julio; de Simoni, Deborah; Aparicio, Ricardo; Coelho, Fernando; Acta Crystallographica Section E 70 (2014) o1200–o1201; doi:10.1107/S1600536814023277

data_2240139
_publ_section_title
;
 Crystal structure of
 3-methoxycarbonyl-2-(4-methoxyphenyl)-8-oxo-1-azaspiro[4.5]deca-1,6,9-trien-1-ium-1-olate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1200
_journal_page_last               o1201
_journal_paper_doi               10.1107/S1600536814023277
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C18 H17 N O5'
_chemical_formula_moiety         'C18 H17 N O5'
_chemical_formula_sum            'C18 H17 N O5'
_chemical_formula_weight         327.32
_chemical_name_systematic
3-Methoxycarbonyl-2-(4-methoxyphenyl)-8-oxo-1-azaspiro[4.5]deca-1,6,9-trien-1-ium-1-olate
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                80.255(6)
_cell_angle_beta                 81.703(6)
_cell_angle_gamma                80.122(6)
_cell_formula_units_Z            2
_cell_length_a                   6.0916(11)
_cell_length_b                   8.7713(16)
_cell_length_c                   15.167(3)
_cell_measurement_reflns_used    109
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.4
_cell_measurement_theta_min      9.0
_cell_volume                     781.3(3)
_computing_cell_refinement
;
SAINT (Bruker, 2010)
;
_computing_data_collection
;
APEX2 (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
<i>WinGX</i> (Farrugia, 2012) and <i>PLATON</i> (Spek, 2009)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14656
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.698
_diffrn_reflns_theta_min         2.977
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.347
_refine_ls_extinction_coef       0.043(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2014)
;
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.3281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                2727
_reflns_number_total             2771
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7301sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        781.3(2)
_cod_database_code               2240139
_cod_database_fobs_code          2240139
_shelx_estimated_absorpt_t_min   0.691
_shelx_estimated_absorpt_t_max   0.869
_shelx_hkl_checksum              35723
_shelx_res_checksum              87745
_shelxl_version_number           2.014