Intercluster Compound between a Tetrakis{triphenylphosphinegold(I)}oxonium Cation and a Keggin Polyoxometalate (POM): Formation during the Course of Carboxylate Elimination of a Monomeric Triphenylphosphinegold(I) Carboxylate in the Presence of POMs
Kenji Nomiya; Takuya Yoshida; Yoshitaka Sakai; Arisa Nanba; Shinichiro Tsuruta; Inorganic Chemistry 49 (2010) 8247–8254; doi:10.1021/ic100530h

data_4316484
_publ_section_title
;
 Intercluster Compound between a
 Tetrakis{triphenylphosphinegold(I)}oxonium Cation and a Keggin
 Polyoxometalate (POM): Formation during the Course of Carboxylate
 Elimination of a Monomeric Triphenylphosphinegold(I) Carboxylate in the
 Presence of POMs
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8247
_journal_page_last               8254
_journal_paper_doi               10.1021/ic100530h
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C224 H204 Au12 O87 P14 W24'
_chemical_formula_weight         11497.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   53.192(5)
_cell_length_b                   53.192(5)
_cell_length_c                   17.100(3)
_cell_measurement_reflns_used    8598
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.27
_cell_volume                     41901(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0882
_diffrn_reflns_av_sigmaI/netI    0.0933
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_h_min       -70
_diffrn_reflns_limit_k_max       70
_diffrn_reflns_limit_k_min       -70
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            113869
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         0.77
_exptl_absorpt_coefficient_mu    16.262
_exptl_absorpt_correction_T_max  0.4420
_exptl_absorpt_correction_T_min  0.1394
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    2.734
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             31068
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         11.013
_refine_diff_density_min         -2.169
_refine_diff_density_rms         0.400
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1074
_refine_ls_number_reflns         21612
_refine_ls_number_restraints     726
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1011P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1613
_refine_ls_wR_factor_ref         0.1723
_reflns_number_gt                14722
_reflns_number_total             21612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100530h_si_002.cif
_cod_data_source_block           ty04s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        41902(10)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4316484