Controlling the Cleavage of Carbon-Carbon Bonds To Generate α,α-Difluorobenzyl Carbanions for the Construction of Difluoromethylbenzenes.
Khatri, Hari R.; Han, Changho; Luong, Erica; Pan, Xiaoliang; Adam, Amna T.; Alshammari, Maali D.; Shao, Yihan; Colby, David A.; The Journal of organic chemistry 84 (2019) 11665–11675; doi:10.1021/acs.joc.9b01595

data_4034462
_publ_section_title
;
 Controlling the Cleavage of Carbon-Carbon Bonds To Generate
 \a,\a-Difluorobenzyl Carbanions for the Construction of
 Difluoromethylbenzenes.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11665
_journal_page_last               11675
_journal_paper_doi               10.1021/acs.joc.9b01595
_journal_volume                  84
_journal_year                    2019
_chemical_formula_sum            'C9 H6 F5 N O4'
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_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
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_atom_sites_solution_primary     direct
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_cell_angle_beta                 90
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_cell_length_c                   19.2501(5)
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_cell_measurement_temperature    150(2)
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_cell_measurement_theta_min      1
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_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius Collect (Nonius, 1998)'
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_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev946 (H\"ubschle et al., 2011)
;
_computing_structure_solution
;
 Direct methods (SIR2004, Burla et al., 2005)
;
_diffrn_ambient_temperature      150(2)
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_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_Laue_measured_fraction_max 0.996
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_min         2.116
_diffrn_source                   'fine focus X-ray tube'
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.9424
_exptl_absorpt_correction_T_min  0.8570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       needle
_exptl_crystal_F_000             1152
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0536P)^2^+0.6866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                2047
_reflns_number_total             2476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b01595_si_002.cif
_cod_data_source_block           ch87
_cod_database_code               4034462
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.943
_shelx_res_checksum              40198
_shelx_hkl_checksum              64046