Stabilization of the P(CF~3~)~2~^-^- Ion as a Reversible CS2Adduct, [P(CF~3~)~2~CS~2~]^-^, and Its Potential Use as a Nucleophilic P(CF~3~)~2~^-^ Source: Synthesis and Structure of [18-crown-6-K][P(C~6~F~5~)~2~CS~2~]
Berthold Hoge; Christoph Thösen; Tobias Herrmann; Ingo Pantenburg; Inorganic Chemistry 41 (2002) 2260–2265; doi:10.1021/ic0112950

data_4317899
_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~^-^- Ion as a Reversible CS2Adduct,
 [P(CF~3~)~2~CS~2~]^-^, and Its Potential Use as a Nucleophilic
 P(CF~3~)~2~^-^ Source: Synthesis and Structure of
 [18-crown-6-K][P(C~6~F~5~)~2~CS~2~]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2260
_journal_page_last               2265
_journal_paper_doi               10.1021/ic0112950
_journal_volume                  41
_journal_year                    2002
_chemical_formula_structural     '[18-crown-6-K][P(C~6~F~5~)~2~CS~2~]'
_chemical_formula_sum            'C26 H26 Cl2 F10 K O6 P S2'
_chemical_formula_weight         829.56
_chemical_name_systematic
;
  18-crown-6-potassium bis(pentafluorophenyl)phosphanodithioformate
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 102.579(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5177(13)
_cell_length_b                   14.981(2)
_cell_length_c                   20.182(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3398.7(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      293(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  0.1214
_diffrn_reflns_av_sigmaI/netI    0.0978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26677
_diffrn_reflns_theta_max         24.07
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.928
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         5227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_obs          0.0666
_refine_ls_shift/esd_max         -0.060
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0999P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1688
_refine_ls_wR_factor_obs         0.1525
_reflns_number_observed          3071
_reflns_number_total             5227
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0112950.cif
_cod_data_source_block           P(CS2)(C6F5)2.18C6.CH2Cl2_in_P21/n
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0999P)^2^+0.0000P] 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^)+(0.0999P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4317899