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_4313737
_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            'C7 H F6 O5 P W'
_chemical_formula_weight         493.90
_chemical_name_common            '[W(CO)5PH(CF3)2]'
_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
_cell_angle_alpha                77.22(2)
_cell_angle_beta                 89.87(2)
_cell_angle_gamma                67.98(2)
_cell_formula_units_Z            2
_cell_length_a                   6.613(2)
_cell_length_b                   7.084(2)
_cell_length_c                   15.455(4)
_cell_measurement_temperature    260(2)
_cell_volume                     652.0(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      260(2)
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0944
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_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            7571
_diffrn_reflns_theta_max         29.58
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    9.069
_exptl_absorpt_correction_T_max  0.4299
_exptl_absorpt_correction_T_min  0.1175
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    2.516
_exptl_crystal_F_000             452
_refine_diff_density_max         1.148
_refine_diff_density_min         -2.183
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0.0078(6)
_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_all   0.799
_refine_ls_goodness_of_fit_obs   0.949
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.800
_refine_ls_restrained_S_obs      0.949
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_obs          0.0356
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0749
_refine_ls_wR_factor_obs         0.0653
_reflns_number_observed          1965
_reflns_number_total             3492
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic034166nsi20030214_121107.cif
_cod_data_source_block           WPHCF3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0344P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        651.9(3)
_cod_database_code               4313737