Preparation and NMR Spectra of Difluoromethylated Silver(I) and Silver(III) Compounds. Structure of [PNP][Ag(CF~2~H)~4~].
Reint Eujen; Berthold Hoge; David J. Brauer; Inorganic Chemistry 36 (1997) 3160–3166; doi:10.1021/ic961398w

data_4323491
_publ_contact_author
;
       Prof. David J. Brauer
       Anorganische Chemie, Fachbereich 9      
       Bergische Universit\"at Gesamthochschule
       Gauszstr. 20
       42097 Wuppertal
       Bundesrepublik Deutschland
;
_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
;
 Preparation and NMR Spectra of Difluoromethylated Silver(I) and
 Silver(III) Compounds. Structure of [PNP][Ag(CF~2~H)~4~].
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3160
_journal_page_last               3166
_journal_paper_doi               10.1021/ic961398w
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        'current publication'
_chemical_formula_moiety         'C36 H30 N P2 +, C4 H4 Ag F8 -'
_chemical_formula_structural     '[(C6 H5)3P]2 N +, Ag(CF2 H)4 -'
_chemical_formula_sum            'C40 H34 Ag F8 N P2'
_chemical_formula_weight         850.49
_chemical_melting_point          394.15
_chemical_name_systematic
; 
 Bis-(triphenylphospnoranyliden)ammonium tetrakis-difluoromethylargentate(III) 
;
_space_group_IT_number           78
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   geom
_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                   9.4748(10)
_cell_length_b                   9.4748(10)
_cell_length_c                   42.159(6)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      32.9
_cell_measurement_theta_min      31.1
_cell_volume                     3784.7(8)
_computing_cell_refinement       'Siemens P3/P4 V4.27'
_computing_data_collection       'Siemens P3/P4 V4.27'
_computing_data_reduction        'Siemens XDISK/XPREP(SHELXTL-PC Version 5)'
_computing_molecular_graphics    'Siemens XP( SHELXTL-PC Version 5'
_computing_publication_material  'SHELXTL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      297(2)
_diffrn_measurement_device       'Siemens P3'
_diffrn_measurement_method       '2\q/\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4038
_diffrn_reflns_theta_max         69.12
_diffrn_reflns_theta_min         4.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.679
_exptl_absorpt_correction_T_max  0.3772
_exptl_absorpt_correction_T_min  0.2468
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            tan
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    none
_exptl_crystal_description       'tetragonal bipyramid'
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(11)
_refine_ls_extinction_coef       0.00076(11)
_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   1.008
_refine_ls_goodness_of_fit_obs   1.019
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         3595
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_restrained_S_obs      1.019
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_obs          0.0453
_refine_ls_shift/esd_max         0.113
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1171
_refine_ls_wR_factor_obs         0.1155
_reflns_number_observed          3444
_reflns_number_total             3595
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961398w.cif
_cod_data_source_block           pnpag
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '121_C' was changed to '394.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+5.0000P] 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^)+(0.0700P)^2^+5.0000P] 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        3784.7(6)
_cod_database_code               4323491