Synthesis of novel angular spirocyclic azetidines.
Guérot, Carine; Tchitchanov, Boris H.; Knust, Henner; Carreira, Erick M.; Organic letters 13 (2011) 780–783; doi:10.1021/ol103050c

data_1501955
_publ_section_title
;
 Synthesis of novel angular spirocyclic azetidines.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              780
_journal_page_last               783
_journal_paper_doi               10.1021/ol103050c
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C19 H19 N O'
_chemical_formula_weight         277.35
_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                95.84(3)
_cell_angle_beta                 99.81(3)
_cell_angle_gamma                110.54(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1910(16)
_cell_length_b                   9.4560(19)
_cell_length_c                   10.496(2)
_cell_measurement_temperature    89(2)
_cell_volume                     738.6(3)
_computing_cell_refinement       XDS
_computing_data_collection       MAR
_computing_data_reduction        XDS
_computing_molecular_graphics    XSHELL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      89(2)
_diffrn_detector_area_resol_mean 0.85
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       Rotation
_diffrn_radiation_source         'SLS-Beamline X10SA'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8298
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.89(5)
_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   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0872P)^2^+0.2573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                2292
_reflns_number_total             2298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol103050c_si_002.cif
_cod_data_source_block           x2037sls
_cod_depositor_comments
;
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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        738.5(3)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               1501955