Heterobimetallic Complexes of Gold(I) with the Tetrathiovanadate Anion. Crystal Structure of [VS4(AuPPh3)2{Au(PPh3)2}]
Fernando Canales; M. Concepción Gimeno; Antonio Laguna; Inorganic Chemistry 37 (1998) 5376–5379; doi:10.1021/ic9712939

data_4323039
_publ_section_title
;
 Heterobimetallic Complexes of Gold(I) with the Tetrathiovanadate Anion.
 Crystal Structure of [VS4(AuPPh3)2{Au(PPh3)2}]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5376
_journal_page_last               5379
_journal_paper_doi               10.1021/ic9712939
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C72 H60 Au3 P4 S4 V'
_chemical_formula_weight         1819.16
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 129.466(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.110(6)
_cell_length_b                   13.087(2)
_cell_length_c                   20.620(3)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      3
_cell_volume                     6689(2)
_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       theta-2theta
_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  0.0804
_diffrn_reflns_av_sigmaI/netI    0.1261
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8076
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.956
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       plate
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.836
_refine_ls_goodness_of_fit_obs   0.982
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4088
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      0.914
_refine_ls_restrained_S_obs      0.932
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_obs          0.0399
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0133P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0814
_refine_ls_wR_factor_obs         0.0662
_reflns_number_observed          2595
_reflns_number_total             4097
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9712939.cif
_cod_data_source_block           concha4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (20 times).

'_geom_angle_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (47
times).

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0133P)^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^)+(0.0133P)^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 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Heavy-atom method' was changed
to 'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        6689.4(19)
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_database_code               4323039