Structure of 8-(4-acetylphenyl)-1,4-dioxa-8-azaspiro[4,5]decane: a new potential nonlinear optical material
Ogawa, Keiichiro; Kaji, Makoto; Kagawa, Hiroyuki; Sagawa, Masakazu; Kakuta, Atsushi; Acta Crystallographica Section C 50 (1994) 95–97; doi:10.1107/S0108270193007917

data_2009390
_publ_contact_author
;
       Prof Keiichiro Ogawa
       Department of Chemistry
       The College of Arts and Sciences,
       The University of Tokyo
       Komaba
       Meguro-ku
       Tokyo
       153 Japan
;
_publ_section_title
;
 Structure of 8-(4-acetylphenyl)-1,4-dioxa-8-azaspiro[4,5]decane: a new
 potential nonlinear optical material
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              95
_journal_page_last               97
_journal_paper_doi               10.1107/S0108270193007917
_journal_volume                  50
_journal_year                    1994
_chemical_formula_analytical     'C15 H19 N O3'
_chemical_formula_moiety         'C15 H19 N O3'
_chemical_formula_sum            'C15 H19 N O3'
_chemical_formula_weight         261.32
_chemical_melting_point          396.5(5)
_chemical_name_common            APDA
_chemical_name_systematic
'       8-(4-Acetylphenyl)-1,4-dioxa-8-azaspiro[4.5]decane'
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8750(10)
_cell_length_b                   9.0360(10)
_cell_length_c                   21.676(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      39.81
_cell_measurement_theta_min      36.74
_cell_volume                     1346.6(3)
_computing_cell_refinement       MSC/AFC
_computing_data_collection
;
  MSC/AFC (Rigaku Corporation, 1988)
;
_computing_data_reduction
;
  Xtal3.0 DIFDAT, ADDREF, SORTRF (Hall & Stewart, 1990)
;
_computing_molecular_graphics
;
  Xtal ORTEP (Johnson, 1965); MindTool (Tirado-Rives & Blake, 1990)
;
_computing_publication_material  'Xtal BONDLA, CIFIO'
_computing_structure_refinement
;
  Xtal3.2 CRYLSQ (Hall, Flack & Stewart, 1992)
;
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Rigaku AFC-6A'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         Cu
_diffrn_radiation_type           xray_tube
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  .009
_diffrn_reflns_av_sigmaI/netI    .005
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1067
_diffrn_reflns_reduction_process 'perpendicular monochr Lp'
_diffrn_reflns_theta_max         60
_diffrn_reflns_theta_min         4.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.69
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'Absorption correction not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_meas      1.295(8)
_exptl_crystal_density_method    'flotation in aqueous KBr solution'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             560(?)
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         .244
_refine_diff_density_min         -.480
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   3.504
_refine_ls_goodness_of_fit_obs   3.575
_refine_ls_hydrogen_treatment    'H atoms not restrained'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     247
_refine_ls_number_reflns         1000
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .052
_refine_ls_R_factor_obs          .051
_refine_ls_shift/esd_max         .201
_refine_ls_shift/esd_mean        .033
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F) + 0.0002F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .067
_refine_ls_wR_factor_obs         .067
_reflns_number_observed          1000
_reflns_number_total             1034
_reflns_observed_criterion       I~net~>2.000\s(I~net~)
_cod_data_source_file            hl1039.cif
_cod_data_source_block           hi0100
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '396-397' was changed to '396.5(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 '396-397' was changed to '396.5(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:

'_refine_ls_weighting_scheme' value '1/[\s^2^(F) + 0.0002F^2^]' 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^(F) +
0.0002F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1346.5(3)
_cod_original_formula_sum        'C15 H19 N1 O3'
_cod_database_code               2009390