Stabilization of the P(CF~3~)~2~^-^ and P(C~6~F~5~)~2~^-^ Ions by Coordination to Pentacarbonyl Tungsten: Structures of [18-crown-6-K]P(CF~3~)~2~, [18-crown-6-K][W{P(CF~3~)~2~}(CO)~5~] and [18-crown-6-K][{W(CO)~5~}~2~{μ-P(C~6~F~5~)~2~}].THF
Berthold Hoge; Christoph Thösen; Tobias Herrmann; Ingo Pantenburg; Inorganic Chemistry 42 (2003) 3633–3641; doi:10.1021/ic034165v

data_4313733
_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
;
 Stabilization of the P(CF~3~)~2~^-^ and P(C~6~F~5~)~2~^-^ Ions by
 Coordination to Pentacarbonyl Tungsten: Structures of
 [18-crown-6-K]P(CF~3~)~2~, [18-crown-6-K][W{P(CF~3~)~2~}(CO)~5~] and
 [18-crown-6-K][{W(CO)~5~}~2~{\m-P(C~6~F~5~)~2~}].THF
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3633
_journal_page_last               3641
_journal_paper_doi               10.1021/ic034165v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C38 H32 F10 K O17 P W2'
_chemical_formula_weight         1388.41
_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                81.961(10)
_cell_angle_beta                 87.452(10)
_cell_angle_gamma                75.429(10)
_cell_formula_units_Z            2
_cell_length_a                   9.1723(11)
_cell_length_b                   15.560(2)
_cell_length_c                   17.007(2)
_cell_measurement_reflns_used    12840
_cell_measurement_temperature    170(2)
_cell_volume                     2326.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0845
_diffrn_reflns_av_sigmaI/netI    0.1068
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30062
_diffrn_reflns_theta_full        27.29
_diffrn_reflns_theta_max         27.29
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    5.175
_exptl_absorpt_correction_T_max  0.6236
_exptl_absorpt_correction_T_min  0.3604
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.683
_refine_diff_density_min         -2.163
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.00203(12)
_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   0.824
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         10320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.824
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0403P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                5988
_reflns_number_total             10320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034165vsi20030214_094442_2.cif
_cod_data_source_block           w2pc6f5
_cod_database_code               4313733