Synthesis, X-ray and solid state NMR studies on silver(I) silanethiolates. Crystal structure of bis[(triphenylphosphine)(tri-o-tolylsilanethiolato)silver(I)]‒toluene(1/2), [{Ag[SSi(C6H4Me-o)3](PPh3)}2]·2C6H5Me †
Chojnacki, Jaroslaw; Becker, Barbara; Konitz, Atoni; Potrzebowski, Marek J.; Wojnowski, Wieslaw; Journal of the Chemical Society, Dalton Transactions  (1999) 3063–; doi:10.1039/a903694f

data_7027535
_publ_contact_author             'Barbara Becker'
_publ_section_title
;
 Synthesis, X-ray and solid state NMR studies on silver(I)
 silanethiolates. Crystal structure of
 bis[(triphenylphosphine)(tri-o-tolylsilanethiolato)silver(I)]--toluene(1/2),
 [{Ag[SSi(C6H4Me-o)3](PPh3)}2]&#x00B7;2C6H5Me&#x200A;&#x2020;
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3063
_journal_paper_doi               10.1039/a903694f
_journal_year                    1999
_chemical_formula_sum            'C46 H44 Ag P S Si'
_chemical_formula_weight         795.80
_chemical_name_systematic
; 
 bis{tri-o-tolylsilanethiolato(tri-phenylphosphine)silver(I)}bis(toluene) 
;
_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           'manual editing of form.cif'
_cell_angle_alpha                115.15(3)
_cell_angle_beta                 99.76(3)
_cell_angle_gamma                107.71(3)
_cell_formula_units_Z            2
_cell_length_a                   12.824(3)
_cell_length_b                   13.667(3)
_cell_length_c                   14.524(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      1.65
_cell_volume                     2059.0(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.673
_diffrn_measured_fraction_theta_max 0.673
_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  0.0154
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8352
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        27.6
_exptl_absorpt_coefficient_mu    0.638
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         8063
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.2120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                4436
_reflns_number_total             8063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903694fsup1.cif
_cod_data_source_block           c090498
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.2120P] 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^)+(0.0487P)^2^+0.2120P] 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        2059.0(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027535