Preparation and NMR Spectra of the (Trifluoromethyl)argentates(III) [Ag(CF~3~)~n~X~4-n~]^-^, with X = CN (n= 1-3), CH~3~, C\τbCC~6~H~11~, Cl, Br (n= 2, 3), and I (n= 3), and of Related Silver(III) Compounds. Structures of [PPh~4~][trans-Ag(CF~3~)~2~(CN)~2~] and [PPh~4~][Ag(CF~3~)~3~CH~3~].
Reint Eujen; Berthold Hoge; David J. Brauer; Inorganic Chemistry 36 (1997) 1464–1475; doi:10.1021/ic9610445

data_4323363
_publ_contact_author
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       Prof. David J. Brauer
       Anorganische Chemie, Fachbereich 9      
       Bergische Universit\"at Gesamthochschule
       Gauszstr. 20
       42097 Wuppertal
       Bundesrepublik Deutschland
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_publ_contact_author_email       brauer@wrcs3.urz.uni-wuppertal.de
_publ_contact_author_fax         '049 202 439-2901'
_publ_contact_author_phone       '049 202 439-2457'
_publ_section_title
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 Preparation and NMR Spectra of the (Trifluoromethyl)argentates(III)
 [Ag(CF~3~)~n~X~4-n~]^-^, with X = CN (n= 1-3), CH~3~, C\\tbCC~6~H~11~,
 Cl, Br (n= 2, 3), and I (n= 3), and of Related Silver(III) Compounds.
 Structures of [PPh~4~][trans-Ag(CF~3~)~2~(CN)~2~] and
 [PPh~4~][Ag(CF~3~)~3~CH~3~].
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1464
_journal_page_last               1475
_journal_paper_doi               10.1021/ic9610445
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        'current publication'
_chemical_formula_moiety         'C24 H20 P 1+, C4 H3 Ag F9 1-'
_chemical_formula_structural     '[P(C6H5)4][Ag(CF3)3CH3]'
_chemical_formula_sum            'C28 H23 Ag F9 P'
_chemical_formula_weight         669.30
_chemical_name_systematic
; 
 Tetraphenylphosphonium tris(trifluoromethyl)methylargenate(III)
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.941(3)
_cell_length_b                   7.2629(6)
_cell_length_c                   14.9985(14)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      34.8
_cell_measurement_theta_min      32.5
_cell_volume                     2716.9(5)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK, SHELXTL XPREP'
_computing_molecular_graphics    'SHELXTL XP'
_computing_publication_material  'SHELXTL XL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measurement_device       'Siemens P3'
_diffrn_measurement_method       '\q/2\q  scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10328
_diffrn_reflns_theta_max         69.10
_diffrn_reflns_theta_min         3.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.228
_exptl_absorpt_correction_T_max  0.47718
_exptl_absorpt_correction_T_min  0.25833
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            tan
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    none
_exptl_crystal_description       rod
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.347(9)
_refine_ls_extinction_coef       0.00121(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   1.043
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5066
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_obs          0.0320
_refine_ls_shift/esd_max         -0.016
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0824
_refine_ls_wR_factor_obs         0.0785
_reflns_number_observed          4374
_reflns_number_total             5066
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9610445_2.cif
_cod_data_source_block           agf3h
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.6000P] 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^)+(0.0400P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        2716.8(4)
_cod_database_code               4323363