Triethylammonium 8-acetyl-3-methyl-9-phenyl-7-oxo-2-azaspiro[4.5]dec-2-ene-4-nitronate
Mauro F.A. Adamo; Stefano Chimichi; Donato Donati; Piero Sarti-Fantoni; Acta Crystallographica Section E 58 (2002) o1125–o1127; doi:10.1107/S1600536802016598

data_2201421
_publ_section_title
;
 Triethylammonium
 8-acetyl-3-methyl-9-phenyl-7-oxo-2-azaspiro[4.5]dec-2-ene-4-nitronate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1125
_journal_page_last               o1127
_journal_paper_doi               10.1107/S1600536802016598
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C17 H17 N2 O5 , C6 H16 N'
_chemical_formula_sum            'C23 H33 N3 O5'
_chemical_formula_weight         431.52
_chemical_melting_point          428
_chemical_name_systematic
;
Triethylammonium 8-Acetyl-3-methyl-9-phenyl-7-oxo-2-azaspiro
[4.5]dec-2-en-4-nitronate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 108.550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.815(3)
_cell_length_b                   10.464(2)
_cell_length_c                   11.222(2)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    293(3)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     2428.6(7)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7207
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' colourless       '
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       ' needles         '
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         3539
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0828P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                2723
_reflns_number_total             3539
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cm6016.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2201421
_cod_database_fobs_code          2201421