Aurophilicity at Sulfur Centers. Synthesis and Reactivity of the Complex [S(Au2dppf)]; Formation of Polynuclear Sulfur-Centered Complexes. Crystal Structures of [S(Au2dppf)].2CHCl3, [(μ-Au2dppf){S(Au2dppf)}2](OTf)2. 8CHCl3, and [S(AuPPh2Me)2(Au2dppf)](ClO4)2.3CH2Cl2
Fernando Canales; M. Concepción Gimeno; Antonio Laguna; Peter G. Jones; Journal of the American Chemical Society 118 (1996) 4839–4845; doi:10.1021/ja9517678

data_4117149
_publ_section_title
;
 Aurophilicity at Sulfur Centers. Synthesis and Reactivity of the Complex
 [S(Au2dppf)]; Formation of Polynuclear Sulfur-Centered Complexes. Crystal
 Structures of [S(Au2dppf)].2CHCl3, [(\m-Au2dppf){S(Au2dppf)}2](OTf)2.
 8CHCl3, and [S(AuPPh2Me)2(Au2dppf)](ClO4)2.3CH2Cl2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4839
_journal_page_last               4845
_journal_paper_doi               10.1021/ja9517678
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C63 H60 Au4 Cl8 Fe O8 P4 S'
_chemical_formula_weight         2228.37
_chemical_name_systematic
;
 ?
;
_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           SHELXL
_cell_angle_alpha                71.738(12)
_cell_angle_beta                 73.264(14)
_cell_angle_gamma                75.96(2)
_cell_formula_units_Z            2
_cell_length_a                   13.727(2)
_cell_length_b                   15.952(3)
_cell_length_c                   17.763(2)
_cell_measurement_reflns_used    66
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5.8
_cell_volume                     3487.3(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w-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  0.1059
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_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            11617
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.067
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_correction_T_min  0.195
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.122
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.936
_refine_diff_density_min         -2.619
_refine_diff_density_rms         0.312
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.086
_refine_ls_goodness_of_fit_obs   1.117
_refine_ls_hydrogen_treatment    riding
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_refine_ls_number_parameters     797
_refine_ls_number_reflns         11506
_refine_ls_number_restraints     1096
_refine_ls_restrained_S_all      1.052
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_obs          0.0768
_refine_ls_shift/esd_max         -0.128
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+127.4682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1945
_refine_ls_wR_factor_obs         0.1570
_reflns_number_observed          7335
_reflns_number_total             11512
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9517678_3.cif
_cod_data_source_block           hurry
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+127.4682P] 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^)+(0.0682P)^2^+127.4682P] 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        3487.5(9)
_cod_database_code               4117149