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_4116557
_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         '(C33 H31 P2 S Au2)2, 2(P F6), 2(H2O)'
_chemical_formula_structural     '[(dppe)2Au4(\m-SC6H4CH3)2](PF6)2'
_chemical_formula_sum            'C66 H66 Au4 F12 O2 P6 S2'
_chemical_formula_weight         2156.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.516(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.0845(3)
_cell_length_b                   13.2873(2)
_cell_length_c                   19.6109(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    270(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.27
_cell_volume                     3638.55(11)
_computing_cell_refinement       'Siemens SMART v4.05'
_computing_data_collection       'Siemens SMART v4.05'
_computing_data_reduction        'Siemens SAINT v4.05'
_computing_molecular_graphics    'Siemens SHELXTL v5.03'
_computing_publication_material  'Siemens SHELXTL v5.03'
_computing_structure_refinement  'Siemens SHELXTL v5.03'
_computing_structure_solution    'Siemens SHELXTL v5.03'
_diffrn_ambient_temperature      270(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  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39496
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        'see exptl_special_details'
_exptl_absorpt_coefficient_mu    8.300
_exptl_absorpt_correction_T_max  0.203568
_exptl_absorpt_correction_T_min  0.074814
_exptl_absorpt_correction_type   'multi-scan (SADABS, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_description       'striated plate'
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.772
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.002
_refine_ls_goodness_of_fit_obs   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         8899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_restrained_S_obs      1.135
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_obs          0.0530
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1476
_refine_ls_wR_factor_obs         0.1277
_reflns_number_observed          5390
_reflns_number_total             8901
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja991986j_2.cif
_cod_data_source_block           98043s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0807P)^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^)+(0.0807P)^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               4116557