Expanding the azaspiro[3.3]heptane family: synthesis of novel highly functionalized building blocks.
Burkhard, Johannes A.; Guérot, Carine; Knust, Henner; Carreira, Erick M.; Organic letters 14 (2012) 66–69; doi:10.1021/ol2028459

data_1503488
_publ_section_title
;
 Expanding the azaspiro[3.3]heptane family: synthesis of novel highly
 functionalized building blocks.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              66
_journal_page_last               69
_journal_paper_doi               10.1021/ol2028459
_journal_volume                  14
_journal_year                    2012
_chemical_compound_source        'LOC ETH Zurich'
_chemical_formula_moiety         'C19 H20 N2 O3 S '
_chemical_formula_sum            'C19 H20 N2 O3 S'
_chemical_formula_weight         356.444
_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'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           maXus
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9856(8)
_cell_length_b                   9.6020(3)
_cell_length_c                   9.2975(3)
_cell_measurement_reflns_used    11301
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1784.21(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.05797
_diffrn_orient_matrix_UB_12      -0.08113
_diffrn_orient_matrix_UB_13      -0.04033
_diffrn_orient_matrix_UB_21      0.06269
_diffrn_orient_matrix_UB_22      0.06835
_diffrn_orient_matrix_UB_23      -0.04738
_diffrn_orient_matrix_UB_31      0.02948
_diffrn_orient_matrix_UB_32      0.00097
_diffrn_orient_matrix_UB_33      0.04042
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3895
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             752.0
_exptl_crystal_size_max          .33
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .21
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.43(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         3715
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.816
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                2973
_reflns_number_total             3715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol2028459_si_002.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 n a 21      '
_cod_original_formula_sum        'C19 H20 N2 O3 S '
_cod_database_code               1503488