Polyoxometalate-Gold(I)/H+ Complexes: Air-Stable, Efficient, Polyvalent, and Bifunctional Catalysts
Hueber, Damien; Hoffmann, Marie; de Frémont, Pierre; Pale, Patrick; Blanc, Aurélien; Organometallics 34 (2015) 5065–; doi:10.1021/acs.organomet.5b00656

data_4087860
_publ_section_title
;
 Polyoxometalate-Gold(I)/H+ Complexes: Air-Stable, Efficient, Polyvalent,
 and Bifunctional Catalysts
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5065
_journal_paper_doi               10.1021/acs.organomet.5b00656
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'O40 Si W12, 4(C5 H12 Au N P), 4(C2 H3 N)'
_chemical_formula_sum            'C28 H60 Au4 N8 O40 P4 Si W12'
_chemical_formula_weight         4294.87
_chemical_name_common            '[(PMe)3Au(MeCN)]4-(POM)2'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 130.0020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.1463(4)
_cell_length_b                   12.7690(2)
_cell_length_c                   23.6131(5)
_cell_measurement_reflns_used    24529
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3729.27(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'Sir 97'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1140
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34092
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.526
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    26.438
_exptl_absorpt_correction_T_max  0.0229
_exptl_absorpt_correction_T_min  0.0031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.825
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3764
_exptl_crystal_recrystallization_method Acetonitrile
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.491
_refine_diff_density_min         -1.837
_refine_diff_density_rms         0.354
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         7336
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+17.4215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6304
_reflns_number_total             7336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00656_si_007.cif
_cod_data_source_block           compound_5a
_cod_original_cell_volume        3729.27(14)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4087860
_shelxl_version_number           2014/6
_shelx_res_checksum              90777
_shelx_hkl_checksum              74760