Electrophilic Fluoroalkylation of Ni(II) N-Confused Porphyrins with Fluoroalkylarylsulfonium Salts
Fei Hao; Hua-Wei Jiang; Guoqiang Zong; Zhiguo Zhou; Ruo-Bing Du; Qing-Yun Chen; Ji-Chang Xiao; Journal of Organic Chemistry 77 (2012) 3604–3608; doi:10.1021/jo3000018

data_4027108
_publ_section_title
;
 Electrophilic Fluoroalkylation of Ni(II) N-Confused Porphyrins with
 Fluoroalkylarylsulfonium Salts
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3604
_journal_page_last               3608
_journal_paper_doi               10.1021/jo3000018
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C47 H29 Cl6 F3 N4 Ni'
_chemical_formula_weight         978.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                119.832(4)
_cell_angle_beta                 96.649(6)
_cell_angle_gamma                90.000(6)
_cell_formula_units_Z            2
_cell_length_a                   10.989(4)
_cell_length_b                   15.032(5)
_cell_length_c                   15.109(5)
_cell_measurement_reflns_used    2994
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      48.171
_cell_measurement_theta_min      4.717
_cell_volume                     2145.7(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0827
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11231
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41185
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.169
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         7859
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1221P)^2^+0.1397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1864
_refine_ls_wR_factor_ref         0.2088
_reflns_number_gt                5726
_reflns_number_total             7859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo3000018_si_001.cif
_cod_data_source_block           cd21129
_cod_original_cell_volume        2145.7(12)
_cod_database_code               4027108