Copper-Promoted Sandmeyer Trifluoromethylation Reaction
Jian-Jun Dai; Chi Fang; Bin Xiao; Jun Yi; Jun Xu; Zhao-Jing Liu; Xi Lu; Lei Liu; Yao Fu; Journal of the American Chemical Society 135 (2013) 8436–8439; doi:10.1021/ja404217t

data_4119931
_publ_section_title
;
 Copper-Promoted Sandmeyer Trifluoromethylation Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8436
_journal_page_last               8439
_journal_paper_doi               10.1021/ja404217t
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C19 H13 F3 Fe'
_chemical_formula_weight         354.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 97.321(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.7098(4)
_cell_length_b                   8.8646(6)
_cell_length_c                   11.5586(5)
_cell_measurement_reflns_used    1287
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      67.4435
_cell_measurement_theta_min      3.8525
_cell_volume                     783.52(8)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies)'
_computing_data_collection       'CrysAlisPro (Agilent Technologies)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies)'
_computing_molecular_graphics    'Ortep-3 (L. J. Farrugia, 2001)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean 15.9149
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Gemini S Ultra, Agilent Technologies'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3210
_diffrn_reflns_theta_full        25.22
_diffrn_reflns_theta_max         25.22
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.7559
_exptl_absorpt_correction_T_min  0.7236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1482
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+2.7346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                1228
_reflns_number_total             1482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404217t_si_003.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        783.52(7)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4119931