Two 5-oxa-2,6-diazaspiro[3.4]octan-1-one derivatives from the [3+2] cycloaddition of methylenelactams with nitrones
Chiaroni, Angèle; Riche, Claude; Rigolet, Séverinne; Mélot, Jean-Marie; Vebrel, Joel; Acta Crystallographica Section C 56 (2000) 473–474; doi:10.1107/S010827010000072X

data_2010814
_publ_section_title
;
 Two 5-oxa-2,6-diazaspiro[3.4]octan-1-one derivatives from the [3+2]
 cycloaddition of methylenelactams with nitrones
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              473
_journal_page_last               474
_journal_paper_doi               10.1107/S010827010000072X
_journal_volume                  56
_journal_year                    2000
_chemical_formula_sum            'C25 H22 N2 O4'
_chemical_formula_weight         414.45
_chemical_melting_point          428.5(5)
_chemical_name_systematic
;
7-benzoyl-2-(4-methoxyphenyl)-6-phenyl-5-oxa-2,6-diazaspiro[3.4]octan-1-one
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.92(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.368(5)
_cell_length_b                   19.776(7)
_cell_length_c                   11.484(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.2
_cell_measurement_theta_min      9.6
_cell_volume                     2082(2)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1987)'
_computing_data_reduction        'NONIUS (Riche, 1989) '
_computing_molecular_graphics    'R3M  (Riche, 1983) and ORTEP (Johnson, 1965)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  .043
_diffrn_reflns_av_sigmaI/netI    .061
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6167
_diffrn_reflns_theta_max         66.95
_diffrn_reflns_theta_min         4.47
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .735
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          .36
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .13
_refine_diff_density_max         .212
_refine_diff_density_min         -.189
_refine_ls_extinction_coef       .0026(4)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.013
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          .101
_refine_ls_R_factor_gt           .050
_refine_ls_shift/esd_mean        .002
_refine_ls_shift/su_max          -.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0724P)^2^+0.164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .147
_refine_ls_wR_factor_ref         .120
_reflns_number_gt                2276
_reflns_number_total             3711
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gs1071.cif
_cod_data_source_block           III
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '428-429' was changed to '428.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '428-429' was changed to '428.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0724P)^2^+0.164P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0724P)^2^+0.164P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2010814
_cod_database_fobs_code          2010814