Diastereoselective Synthesis of CF<sub>3</sub>-Containing Vicinal Diamines.
Huang, Qiu-Xia; Zheng, Qu-Tong; Duan, Yaya; Lin, Jin-Hong; Xiao, Ji-Chang; Zheng, Xing; The Journal of organic chemistry 82 (2017) 8273–8281; doi:10.1021/acs.joc.7b01261

data_4037512
_publ_section_title
;
 Diastereoselective Synthesis of CF<sub>3</sub>-Containing Vicinal
 Diamines.
;
_journal_issue                   15
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8273
_journal_page_last               8281
_journal_paper_doi               10.1021/acs.joc.7b01261
_journal_volume                  82
_journal_year                    2017
_chemical_formula_sum            'C19 H20 F3 N O3 S'
_chemical_formula_weight         399.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                97.645(3)
_cell_angle_beta                 97.068(3)
_cell_angle_gamma                96.897(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9029(13)
_cell_length_b                   10.2491(15)
_cell_length_c                   10.8402(16)
_cell_measurement_reflns_used    2139
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      49.034
_cell_measurement_theta_min      5.139
_cell_volume                     963.5(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5722
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.915
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.036(6)
_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   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3722
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+0.2662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.1909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3020
_reflns_number_total             3722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b01261_si_002.cif
_cod_data_source_block           cd214187_5
_cod_database_code               4037512
_shelxl_version_number           2013-4
_shelx_res_checksum              4054
_shelx_hkl_checksum              90560