Stoichiometric and Catalytic Aryl-Perfluoroalkyl Coupling at Tri-tert-butylphosphine Palladium(II) Complexes.
Ferguson, Devin M.; Bour, James R.; Canty, Allan J.; Kampf, Jeff W.; Sanford, Melanie S.; Journal of the American Chemical Society 139 (2017) 11662–11665; doi:10.1021/jacs.7b05216

data_4131425
_publ_section_title
;
 Stoichiometric and Catalytic Aryl-Perfluoroalkyl Coupling at
 Tri-tert-butylphosphine Palladium(II) Complexes.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11662
_journal_page_last               11665
_journal_paper_doi               10.1021/jacs.7b05216
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C20 H32 F5 P Pd'
_chemical_formula_sum            'C20 H32 F5 P Pd'
_chemical_formula_weight         504.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
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_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   14.39046(10)
_cell_length_c                   18.03556(14)
_cell_measurement_reflns_used    44062
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      69.1120
_cell_measurement_theta_min      4.7110
_cell_volume                     4361.93(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
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_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            64362
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.434
_diffrn_reflns_theta_min         4.730
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    7.958
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       plate
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+3.4928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4057
_reflns_number_total             4073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b05216_si_003.cif
_cod_data_source_block           dmf4178
_cod_database_code               4131425
_shelx_estimated_absorpt_t_min   0.402
_shelx_estimated_absorpt_t_max   0.606
_shelxl_version_number           2014/6
_shelx_res_checksum              85453
_shelx_hkl_checksum              8824