Enantioselective Bromoaminocyclization Using Amino-Thiocarbamate Catalysts
Ling Zhou; Jie Chen; Chong Kiat Tan; Ying-Yeung Yeung; Journal of the American Chemical Society 133 (2011) 9164–9167; doi:10.1021/ja201627h

data_4106276
_publ_section_title
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 Enantioselective Bromoaminocyclization Using Amino-Thiocarbamate
 Catalysts
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9164
_journal_page_last               9167
_journal_paper_doi               10.1021/ja201627h
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C17 H17 Br N2 O4 S'
_chemical_formula_weight         425.30
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_atom_sites_solution_secondary   difmap
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_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6979(9)
_cell_length_b                   31.650(4)
_cell_length_c                   7.1103(8)
_cell_measurement_reflns_used    893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.28
_cell_volume                     1732.3(4)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       9
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_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12209
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    2.519
_exptl_absorpt_correction_T_max  0.7194
_exptl_absorpt_correction_T_min  0.4037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.973
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.026(10)
_refine_ls_extinction_method     none
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_refine_ls_number_parameters     226
_refine_ls_number_reflns         3953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                3532
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201627h_si_001.cif
_cod_data_source_block           a617a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_original_cell_volume        1732.3(3)
_cod_database_code               4106276