Construction of Multifunctional Modules for Drug Discovery: Synthesis of Novel Thia/Oxa-Azaspiro[3.4]octanes.
Li, Dong Bo; Rogers-Evans, Mark; Carreira, Erick M.; Organic letters 15 (2013) 4766–4769; doi:10.1021/ol402127b

data_1512329
_publ_section_title
;
 Construction of Multifunctional Modules for Drug Discovery: Synthesis of
 Novel Thia/Oxa-Azaspiro[3.4]octanes.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4766
_journal_page_last               4769
_journal_paper_doi               10.1021/ol402127b
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C18 H24 Br N3 O4'
_chemical_formula_sum            'C18 H24 Br N3 O4'
_chemical_formula_weight         426.31
_space_group_IT_number           1
_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                83.60(8)
_cell_angle_beta                 88.96(7)
_cell_angle_gamma                80.16(5)
_cell_formula_units_Z            2
_cell_length_a                   5.720(8)
_cell_length_b                   11.095(18)
_cell_length_c                   15.48(3)
_cell_measurement_reflns_used    2454
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      62.9
_cell_measurement_theta_min      4.09
_cell_volume                     962(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Platon, Ortep'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement
'OLEX2 (Dolomanov, 2009), SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Incoatec I\S microfocus X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7876
_diffrn_reflns_theta_full        64.22
_diffrn_reflns_theta_max         64.22
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    3.154
_exptl_absorpt_correction_T_max  0.9937
_exptl_absorpt_correction_T_min  0.7034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.677
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         3731
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.005
_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          0.1639
_refine_ls_wR_factor_ref         0.1737
_reflns_number_gt                3037
_reflns_number_total             3731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol402127b_si_002.cif
_cod_data_source_block           cu_ca040112_0m
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P1
_cod_database_code               1512329