Stereoselective Construction of Bridged trans-aza-Bicyclo[7/6,3/2,1]alkenyl Imines through Ring Expansion aza-Cope Rearrangement.
Shen, Mei-Hua; Xu, Ke; Sun, Chu-Han; Xua, Hua-Dong; Organic letters 17 (2015) 5598–5601; doi:10.1021/acs.orglett.5b02798

data_1540610
_publ_section_title
;
 Stereoselective Construction of Bridged
 trans-aza-Bicyclo[7/6,3/2,1]alkenyl Imines through Ring Expansion
 aza-Cope Rearrangement.
;
_journal_issue                   22
_journal_name_full               'Organic letters'
_journal_page_first              5598
_journal_page_last               5601
_journal_paper_doi               10.1021/acs.orglett.5b02798
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C23 H30 N2 O4 S'
_chemical_formula_weight         430.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.715(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7796(13)
_cell_length_b                   34.171(6)
_cell_length_c                   8.2694(14)
_cell_measurement_reflns_used    2444
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.90
_cell_measurement_theta_min      2.38
_cell_volume                     2193.7(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12025
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.9615
_exptl_absorpt_correction_T_min  0.9530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0064(13)
_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   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3844
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.2189
_refine_ls_R_factor_gt           0.1536
_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^)+(0.0000P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2663
_refine_ls_wR_factor_ref         0.2998
_reflns_number_gt                2057
_reflns_number_total             3844
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol5b02798_si_002.cif
_cod_data_source_block           mo_150521a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               1540610