Bis(trifluoromethyl)phosphane and Bis(pentafluorophenyl)phosphane and Their Pentacarbonyl Tungsten Complexes: Improved Synthesis and an Experimental and Density Functional Study
Berthold Hoge; Tobias Herrmann; Christoph Thösen; Ingo Pantenburg; Inorganic Chemistry 42 (2003) 3623–3632; doi:10.1021/ic034166n

data_4313736
_publ_contact_author_address
;
        Institut f\"ur Anorganische Chemie
        Universit\"at zu K\"oln
        Greinstra\&se 6
        D-50939 K\"oln
        Germany
;
_publ_contact_author_email       b.hoge@uni-koeln.de
_publ_contact_author_fax         '+49 221 470 5196'
_publ_contact_author_name
;
        Dr. B. Hoge
;
_publ_contact_author_phone       '+49 221 470 3911'
_publ_section_title
;
 Bis(trifluoromethyl)phosphane and Bis(pentafluorophenyl)phosphane and
 Their Pentacarbonyl Tungsten Complexes: Improved Synthesis and an
 Experimental and Density Functional Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3623
_journal_page_last               3632
_journal_paper_doi               10.1021/ic034166n
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C17 H F10 O5 P W'
_chemical_formula_weight         690.00
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.36
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.967(2)
_cell_length_b                   7.4776(7)
_cell_length_c                   17.151(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1954.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1000
_diffrn_reflns_av_sigmaI/netI    0.0845
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20001
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    6.116
_exptl_crystal_density_diffrn    2.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1288
_refine_diff_density_max         0.974
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.00039(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   0.825
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.825
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0061P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0411
_refine_ls_wR_factor_ref         0.0453
_reflns_number_gt                2789
_reflns_number_total             4271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034166nsi20030214_121048.cif
_cod_data_source_block           wcop6f5
_cod_original_cell_volume        1954.4(5)
_cod_database_code               4313736