Dual-Organocatalyst-Promoted Asymmetric Cascade Reaction: Highly Efficient Construction of Enantiopure Fully Substituted Tetrahydro-1,2-oxazines.
Lin, Hua; Sun, Xing-Wen; Lin, Guo-Qiang; Organic letters 16 (2014) 752–755; doi:10.1021/ol403463h

data_1513491
_publ_section_title
;
 Dual-Organocatalyst-Promoted Asymmetric Cascade Reaction: Highly
 Efficient Construction of Enantiopure Fully Substituted
 Tetrahydro-1,2-oxazines.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              752
_journal_page_last               755
_journal_paper_doi               10.1021/ol403463h
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration rm
_chemical_formula_sum            'C50 H47 Br2 N3 O5'
_chemical_formula_weight         929.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.863(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.123(4)
_cell_length_b                   10.409(3)
_cell_length_c                   15.834(4)
_cell_measurement_reflns_used    4182
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.89
_cell_measurement_theta_min      2.35
_cell_volume                     2479.5(12)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.1114
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18131
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.29
_diffrn_standards_decay_%        7.35
_exptl_absorpt_coefficient_mu    1.680
_exptl_absorpt_correction_T_max  0.8635
_exptl_absorpt_correction_T_min  0.4585
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.032(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         10959
_refine_ls_number_restraints     331
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0878P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1799
_reflns_number_gt                6648
_reflns_number_total             10959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol403463h_si_002.cif
_cod_data_source_block           mo_20927a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2479.4(10)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               1513491