Synthesis of tert-butyl 6-oxo-2-azaspiro[3.3]heptane-2-carboxylate.
Meyers, Marvin J.; Muizebelt, Inouk; van Wiltenburg, Jim; Brown, David L.; Thorarensen, Atli; Organic letters 11 (2009) 3523–3525; doi:10.1021/ol901325s

data_1504055
_publ_section_title
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 Synthesis of tert-butyl 6-oxo-2-azaspiro[3.3]heptane-2-carboxylate.
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_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              3523
_journal_page_last               3525
_journal_paper_doi               10.1021/ol901325s
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C11 H17 N O3'
_chemical_formula_weight         211.26
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.6040(10)
_cell_angle_beta                 96.856(2)
_cell_angle_gamma                97.248(2)
_cell_formula_units_Z            2
_cell_length_a                   6.6599(2)
_cell_length_b                   9.8956(3)
_cell_length_c                   9.9738(3)
_cell_measurement_reflns_used    2051
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      62.18
_cell_measurement_theta_min      4.75
_cell_volume                     609.01(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.715
_diffrn_measured_fraction_theta_max 0.715
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0129
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2480
_diffrn_reflns_theta_full        62.20
_diffrn_reflns_theta_max         62.20
_diffrn_reflns_theta_min         4.75
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.9731
_exptl_absorpt_correction_T_min  0.8752
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.074(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.192
_refine_ls_shift/su_mean         0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1104P)^2^+0.1030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1544
_reflns_number_gt                1270
_reflns_number_total             1377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol901325s_si_002.cif
_cod_data_source_block           m123
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1504055