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_4313734
_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            'C19 H24 F6 K O11 P W'
_chemical_formula_weight         796.30
_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                75.51(2)
_cell_angle_beta                 70.581(14)
_cell_angle_gamma                88.301(15)
_cell_formula_units_Z            2
_cell_length_a                   10.450(2)
_cell_length_b                   11.398(2)
_cell_length_c                   13.181(3)
_cell_measurement_temperature    170(2)
_cell_volume                     1431.1(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      170(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  0.0932
_diffrn_reflns_av_sigmaI/netI    0.1943
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11971
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    4.327
_exptl_absorpt_correction_T_max  0.6868
_exptl_absorpt_correction_T_min  0.3899
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_F_000             776
_refine_diff_density_max         0.827
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.00009(10)
_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   0.636
_refine_ls_goodness_of_fit_obs   0.678
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         5445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.641
_refine_ls_restrained_S_obs      0.678
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_obs          0.0396
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\s^2^(Fo^2^)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0679
_refine_ls_wR_factor_obs         0.0528
_reflns_number_observed          3101
_reflns_number_total             5461
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic034165vsi20030214_094442_3.cif
_cod_data_source_block           wpcf3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)] ' 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^)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4313734