Spiro[1-azabicyclo[5.3.0]decane-6,2'(5'<i>H</i>)-furan]-5',10-dione: an example of kryptoracemic crystallization
Lynch, Vincent M.; Bur, Scott K.; Martin, Stephen F.; Acta Crystallographica Section C 55 (1999) 622–624; doi:10.1107/S0108270198012748

data_2008353
_publ_contact_author
;
 Dr. Vincent M. Lynch
 Department of Chemistry and Biochemistry
 University of Texas at Austin
 Austin, TX 78712, USA
;
_publ_section_title
;
 Spiro[1-azabicyclo[5.3.0]decane-6,2'(5'<i>H</i>)-furan]-5',10-dione:
 an example of kryptoracemic crystallization
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              622
_journal_page_last               624
_journal_paper_doi               10.1107/S0108270198012748
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C12 H15 N O3'
_chemical_formula_weight         221.25
_chemical_name_systematic
;
Spiro[1-azabicyclo[5.3.0]decane-6,2'(5'H)-furan]-2'10-dione
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.161(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1530(10)
_cell_length_b                   11.4950(10)
_cell_length_c                   10.2770(10)
_cell_measurement_reflns_used    51
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      12.2
_cell_volume                     1079.64(18)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'XP in SHELXTL-Plus'
_computing_structure_refinement  'XL in SHELXTL-Plus'
_computing_structure_solution    'XS in SHELXTL-Plus (Sheldrick, 1994)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5988
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        'less than 1'
_diffrn_standards_interval_count 75
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'cut, triangular prism'
_exptl_crystal_F_000             472
_exptl_crystal_size_max          .7
_exptl_crystal_size_mid          .6
_exptl_crystal_size_min          .5
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.168
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.5(8)
_refine_ls_extinction_coef       0.042(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.006
_refine_ls_goodness_of_fit_obs   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         3526
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.006
_refine_ls_restrained_S_obs      1.015
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_obs          0.0337
_refine_ls_shift/esd_max         -0.012
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w  = 1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.2386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0824
_refine_ls_wR_factor_obs         0.0796
_reflns_number_observed          3263
_reflns_number_total             3526
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fr1145.cif
_cod_data_source_block           da1996
_cod_depositor_comments
;
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^)+(0.0418P)^2^+0.2386P] 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^)+(0.0418P)^2^+0.2386P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1079.6(2)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2008353
_cod_database_fobs_code          2008353