A New Reagent for Direct Difluoromethylation
Yuta Fujiwara; Janice A. Dixon; Rodrigo A. Rodriguez; Ryan D. Baxter; Darryl D. Dixon; Michael R. Collins; Donna G. Blackmond; Phil S. Baran; Journal of the American Chemical Society 134 (2012) 1494–1497; doi:10.1021/ja211422g

data_4117359
_publ_section_title
;
 A New Reagent for Direct Difluoromethylation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1494
_journal_page_last               1497
_journal_paper_doi               10.1021/ja211422g
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C6 H18 F12 O18 S6 Zn3'
_chemical_formula_weight         994.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   9.2688(3)
_cell_length_b                   9.2688(3)
_cell_length_c                   88.532(3)
_cell_measurement_reflns_used    4570
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.80
_cell_measurement_theta_min      4.49
_cell_volume                     6586.9(4)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker SMART 6K CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirror'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1000
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       104
_diffrn_reflns_limit_l_min       -106
_diffrn_reflns_number            22234
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         68.12
_diffrn_reflns_theta_min         5.53
_exptl_absorpt_coefficient_mu    8.292
_exptl_absorpt_correction_T_max  0.7890
_exptl_absorpt_correction_T_min  0.4910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.257
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4428
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.330
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.271
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1826P)^2^+97.9066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2759
_refine_ls_wR_factor_ref         0.3022
_reflns_number_gt                1831
_reflns_number_total             2646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211422g_si_004.cif
_cod_data_source_block           pflj235
_cod_original_cell_volume        6586.8(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4117359