Fundamental Studies and Development of Nickel-Catalyzed Trifluoromethylthiolation of Aryl Chlorides: Active Catalytic Species and Key Roles of Ligand and Traceless MeCN Additive Revealed.
Yin, Guoyin; Kalvet, Indrek; Englert, Ulli; Schoenebeck, Franziska; Journal of the American Chemical Society 137 (2015) 4164–4172; doi:10.1021/jacs.5b00538

data_4123550
_publ_section_title
;
 Fundamental Studies and Development of Nickel-Catalyzed
 Trifluoromethylthiolation of Aryl Chlorides: Active Catalytic Species and
 Key Roles of Ligand and Traceless MeCN Additive Revealed.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4164
_journal_page_last               4172
_journal_paper_doi               10.1021/jacs.5b00538
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C34 H28 Cl Fe Ni P2, C6 H6'
_chemical_formula_sum            'C40 H34 Cl Fe Ni P2'
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_chemical_name_common            'IK_N237 = u14_18'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
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_audit_creation_method           SHELXL-2013
_cell_angle_alpha                96.424(2)
_cell_angle_beta                 104.691(2)
_cell_angle_gamma                104.454(2)
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_cell_length_c                   17.402(2)
_cell_measurement_reflns_used    4168
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.27
_cell_volume                     1679.7(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
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_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'Incoatec microsource'
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_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
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_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_limit_l_min       -21
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.453
_diffrn_reflns_theta_min         2.273
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_exptl_crystal_description       'rod-shaped fragment'
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_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0300P)^2^+0.5000P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
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_reflns_number_total             6906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b00538_si_002.cif
_cod_data_source_block           u14_18
_cod_database_code               4123550
_shelx_estimated_absorpt_t_min   0.762
_shelx_estimated_absorpt_t_max   0.890
_shelxl_version_number           2013-2
_shelx_res_checksum              11765
_shelx_hkl_checksum              47016