Electrochemical and Chemical Oxidation of Gold(I) Thiolate Phosphine Complexes: Formation of Gold Clusters and Disulfide
Jinhua Chen; Tong Jiang; Gang Wei; Ahmed A. Mohamed; Craig Homrighausen; Jeanette A. Krause Bauer; Alice E. Bruce; Mitchell R. M. Bruce; Journal of the American Chemical Society 121 (1999) 9225–9226; doi:10.1021/ja991986j

data_4116556
_publ_contact_author_email       abruce@maine.maine.edu
_publ_contact_author_fax         '207 581 1191'
_publ_contact_author_phone       '207 581 1182'
_publ_section_title
;
 Electrochemical and Chemical Oxidation of Gold(I) Thiolate Phosphine
 Complexes: Formation of Gold Clusters and Disulfide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9225
_journal_page_last               9226
_journal_paper_doi               10.1021/ja991986j
_journal_volume                  121
_journal_year                    1999
_chemical_formula_moiety         '(C43 H37 P2 S Au2)2, 2(P F6)'
_chemical_formula_structural     '[(Ph3P)4Au4(\m-SC6H4CH3)2](PF6)2'
_chemical_formula_sum            'C86 H74 Au4 F12 P6 S2'
_chemical_formula_weight         2373.26
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   18.6416(2)
_cell_length_b                   18.8457(4)
_cell_length_c                   24.1510(4)
_cell_measurement_reflns_used    8006
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.28
_cell_volume                     8484.6(2)
_computing_cell_refinement       'Bruker AXS SMART v5.045'
_computing_data_collection       'Bruker AXS SMART v5.045'
_computing_data_reduction        'Bruker AXS SAINT v5.045'
_computing_molecular_graphics    'Bruker AXS SHELXTL v5.03'
_computing_publication_material  'Bruker AXS SHELXTL v5.03'
_computing_structure_refinement  'Bruker AXS SHELXTL v5.03'
_computing_structure_solution    'Bruker AXS SHELXTL v5.03'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1669
_diffrn_reflns_av_sigmaI/netI    0.1387
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            89962
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        'see exptl_special_details'
_exptl_absorpt_coefficient_mu    7.127
_exptl_absorpt_correction_T_max  0.379059
_exptl_absorpt_correction_T_min  0.266916
_exptl_absorpt_correction_type   'multi-scan (SADABS, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_description       needle
_exptl_crystal_F_000             4544
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.804
_refine_ls_goodness_of_fit_obs   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         10497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.808
_refine_ls_restrained_S_obs      0.985
_refine_ls_R_factor_all          0.1492
_refine_ls_R_factor_obs          0.0365
_refine_ls_shift/esd_max         0.064
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0101P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0498
_refine_ls_wR_factor_obs         0.0376
_reflns_number_observed          4356
_reflns_number_total             10499
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja991986j_1.cif
_cod_data_source_block           98032c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0101P)^2^+0.0000P] 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^)+(0.0101P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116556