Silver(I) Pyrazolates. Synthesis and X-ray and 31P-NMR Characterization of Triphenylphosphine Complexes and Their Reactivity toward Heterocumulenes
G. Attilio Ardizzoia; Girolamo La Monica; Angelo Maspero; Massimo Moret; Norberto Masciocchi; Inorganic Chemistry 36 (1997) 2321–2328; doi:10.1021/ic960908j

data_4323432
_publ_contact_author             'G.Attilio Ardizzoia'
_publ_contact_author_email       attilio@csmtbo.mi.cnr.it
_publ_section_title
;
 Silver(I) Pyrazolates. Synthesis and X-ray and 31P-NMR Characterization
 of Triphenylphosphine Complexes and Their Reactivity toward
 Heterocumulenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2321
_journal_page_last               2328
_journal_paper_doi               10.1021/ic960908j
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C40 H33 Ag N2 P2 S2'
_chemical_formula_weight         775.61
_space_group_IT_number           2
_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                86.71(2)
_cell_angle_beta                 75.14(2)
_cell_angle_gamma                74.79(2)
_cell_formula_units_Z            2
_cell_length_a                   10.329(4)
_cell_length_b                   13.082(2)
_cell_length_c                   14.284(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     1800.1(9)
_computing_molecular_graphics    'ORTEP (Johnson)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD-4
_diffrn_measurement_method       'omega scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6296
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '7200 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          '0.25 mm'
_exptl_crystal_size_mid          '0.20 mm'
_exptl_crystal_size_min          '0.03 mm'
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.035
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_obs          0.0279
_refine_ls_shift/esd_max         0.021
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.7765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0767
_refine_ls_wR_factor_obs         0.0702
_reflns_number_observed          5179
_reflns_number_total             6296
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960908j_3.cif
_cod_data_source_block           Complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.7765P] 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^)+(0.0410P)^2^+0.7765P] 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        1800.1(8)
_cod_database_code               4323432