(2<i>S</i>,3<i>R</i>,4<i>R</i>,5<i>S</i>)-3,4-<i>O</i>-Isopropylidene-2-methyl-1-oxa-6,9-diazaspiro[4.5]decane-7,10-dione
David J. Watkin; Matthias Müller; Yves Blèriot; Michela I. Simone; George W. J. Fleet; Acta Crystallographica Section E 60 (2004) o1820–o1822; doi:10.1107/S1600536804022494

data_2204285
_publ_section_title
(2<i>S</i>,3<i>R</i>,4<i>R</i>,5<i>S</i>)-3,4-<i>O</i>-Isopropylidene-2-methyl-1-oxa-6,9-diazaspiro[4.5]decane-7,10-dione
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1820
_journal_page_last               o1822
_journal_paper_doi               10.1107/S1600536804022494
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C11 H13 N2 O5'
_chemical_formula_moiety         'C11 H13 N2 O5'
_chemical_formula_sum            'C11 H13 N2 O5'
_chemical_formula_weight         253.24
_chemical_name_systematic
;
(2S,3R,4R,5S)-3,4-O-isopropylidene-2-methyl-6,9-diazo-1-oxaspiro
-[4.5]-decane-7,10-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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 93.00(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.100(2)
_cell_length_b                   7.994(2)
_cell_length_c                   13.895(2)
_cell_measurement_reflns_used    5932
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      2.0
_cell_volume                     1231.3(4)
_computing_cell_refinement       'DENZO and SCALEPACK'
_computing_data_collection       'XPRESS (MacScience, 1989)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'Nonius DIP2000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5932
_diffrn_reflns_theta_full        25.234
_diffrn_reflns_theta_max         26.563
_diffrn_reflns_theta_min         1.467
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0722
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         2404
_refine_ls_number_restraints     97
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.003758
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w = 1/[\s^2^(F)+0.034 +0.093P], where P = (max(F~o~^2^,0)+2F~c~^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1392
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                2404
_reflns_number_total             2417
_reflns_threshold_expression     I>-3\s(I)
_cod_data_source_file            cf6370.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               2204285
_cod_database_fobs_code          2204285