Trifluoromethylation of Secondary Nitroalkanes.
Gietter-Burch, Amber A S; Devannah, Vijayarajan; Watson, Donald A.; Organic letters 19 (2017) 2957–2960; doi:10.1021/acs.orglett.7b01196

data_1546097
_publ_section_title
;
 Trifluoromethylation of Secondary Nitroalkanes.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2957
_journal_page_last               2960
_journal_paper_doi               10.1021/acs.orglett.7b01196
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C14 H13 F6 N O2'
_chemical_formula_weight         341.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.9950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   15.0424(12)
_cell_length_b                   9.1167(7)
_cell_length_c                   42.181(3)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.51
_cell_volume                     5741.5(8)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            73145
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.880
_diffrn_reflns_theta_min         1.364
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.575
_exptl_crystal_size_mid          0.477
_exptl_crystal_size_min          0.388
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         15030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+4.9805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10383
_reflns_number_total             15030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b01196_si_001.cif
_cod_data_source_block           donw055
_cod_depositor_comments          'Adding full bibliography for 1546097.cif.'
_cod_database_code               1546097
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.942
_shelx_res_checksum              28875
_shelx_hkl_checksum              88225