A Model for C-F Activation by Electrophilic Phosphonium Cations
Mallov, Ian; Johnstone, Tim; Burns, Darcy; Stephan, Douglas W.; Chem. Commun.  (2017) –; doi:10.1039/C7CC04057A

data_7120264
_publ_section_title
;
 A Model for C-F Activation by Electrophilic Phosphonium Cations
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04057A
_journal_year                    2017
_chemical_formula_sum            'C48 H8 B Cl2 F34 P'
_chemical_formula_weight         1343.22
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.302(7)
_cell_angle_beta                 97.601(7)
_cell_angle_gamma                99.450(8)
_cell_formula_units_Z            4
_cell_length_a                   12.0867(19)
_cell_length_b                   14.713(3)
_cell_length_c                   27.639(5)
_cell_measurement_reflns_used    2700
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.02
_cell_measurement_theta_min      2.63
_cell_volume                     4804.0(15)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_av_unetI/netI     0.1559
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37892
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        24.407
_diffrn_reflns_theta_max         24.407
_diffrn_reflns_theta_min         0.744
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_description       needle
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.362
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1569
_refine_ls_number_reflns         15465
_refine_ls_number_restraints     1649
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.2063
_refine_ls_R_factor_gt           0.0976
_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^)+(0.1619P)^2^+16.5305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2537
_refine_ls_wR_factor_ref         0.3236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7165
_reflns_number_total             15465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04057a2.cif
_cod_data_source_block           new2
_cod_original_cell_volume        4803.8(14)
_cod_database_code               7120264
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.686
_shelx_estimated_absorpt_t_max   0.935
_shelx_res_checksum              94049
_shelx_hkl_checksum              35657