Synthetic, Thermochemical, and Catalytic Studies of Fluorinated Tertiary Phosphine Ligands R2PRf [R = Cy, Ph, iPr; Rf= CH'2CH2(CF2)5CF3] in Rhodium Systems
Dale C. Smith; Edwin D. Stevens; Steven P. Nolan; Inorganic Chemistry 38 (1999) 5277–5281; doi:10.1021/ic990430u

data_4322394
_publ_section_title
;
 Synthetic, Thermochemical, and Catalytic Studies of Fluorinated Tertiary
 Phosphine Ligands R2PRf [R = Cy, Ph, iPr; Rf= CH'2CH2(CF2)5CF3] in
 Rhodium Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5277
_journal_page_last               5281
_journal_paper_doi               10.1021/ic990430u
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C41 H28 Cl F26 O P2 Rh'
_chemical_formula_weight         1230.93
_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                84.180(2)
_cell_angle_beta                 80.976(2)
_cell_angle_gamma                64.847(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1416(8)
_cell_length_b                   12.8890(9)
_cell_length_c                   17.3455(13)
_cell_measurement_reflns_used    2609
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      10.0
_cell_volume                     2424.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART 1k CCD'
_diffrn_measurement_method       '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  0.0871
_diffrn_reflns_av_sigmaI/netI    0.3689
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14026
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62407
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.653
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         8331
_refine_ls_number_restraints     847
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1920
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.243
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.2039
_reflns_number_gt                2929
_reflns_number_total             8331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990430u.cif
_cod_data_source_block           nol31c
_cod_database_code               4322394