Synthesis of α-tribromomethylamines via Mg-mediated addition of bromoform to imines.
Gopi, Elumalai; Namboothiri, Irishi N. N.; Organic & biomolecular chemistry 12 (2014) 2769–2777; doi:10.1039/c4ob00259h

data_7153707
_publ_section_title
;
 Synthesis of \a-tribromomethylamines via Mg-mediated addition of
 bromoform to imines.
;
_journal_issue                   17
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2769
_journal_page_last               2777
_journal_paper_doi               10.1039/c4ob00259h
_journal_volume                  12
_journal_year                    2014
_chemical_formula_moiety         'C18 H18 Br3 N O3 S'
_chemical_formula_sum            'C18 H18 Br3 N O3 S'
_chemical_formula_weight         568.12
_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                 98.985(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.212(3)
_cell_length_b                   11.258(3)
_cell_length_c                   17.747(4)
_cell_measurement_reflns_used    3180
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.1
_cell_volume                     2015.3(9)
_computing_cell_refinement
; 
CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012) 
;
_computing_data_collection
; 
CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012) 
;
_computing_data_reduction
; 
CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012) 
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
; 
Rigaku CrystalClear-SM Expert 2.1 b24 
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         MicroMax003_Mo
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15300
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    6.127
_exptl_absorpt_correction_T_max  0.522
_exptl_absorpt_correction_T_min  0.277
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
Rigaku CrystalClear-SM Expert 2.1 b24 
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                2982
_reflns_number_total             3677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ob00259h3.cif
_cod_data_source_block           shelxl
_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/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Numerical'
changed to 'numerical' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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_sg_symbol_H-M      'P 21/n'
_cod_database_code               7153707