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_4087865
_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
'O62 P2 W18,5(C20 H18 Au N P),4(C2 H3 N),2(O)'
_chemical_formula_sum            'C108 H102 Au5 N9 O64 P7 W18'
_chemical_formula_weight         7060.90
_chemical_name_common            (PPh3)Au(MeCN)POM
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                87.8810(10)
_cell_angle_beta                 77.5690(10)
_cell_angle_gamma                60.6940(10)
_cell_formula_units_Z            2
_cell_length_a                   20.4409(5)
_cell_length_b                   20.5221(5)
_cell_length_c                   20.9542(3)
_cell_measurement_reflns_used    47703
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     7461.2(3)
_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    Superflip
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_unetI/netI     0.0996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            70117
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.357
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    18.864
_exptl_absorpt_correction_T_max  0.0392
_exptl_absorpt_correction_T_min  0.0105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_density_diffrn    3.143
_exptl_crystal_description       Prism
_exptl_crystal_F_000             6314
_exptl_crystal_recrystallization_method Acetonitrile
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.280
_refine_diff_density_min         -3.825
_refine_diff_density_rms         0.355
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1920
_refine_ls_number_reflns         29280
_refine_ls_number_restraints     756
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+44.8509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19599
_reflns_number_total             29280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00656_si_006.cif
_cod_data_source_block           compound_4a
_cod_database_code               4087865
_shelxl_version_number           2014/6
_shelx_res_checksum              49283
_shelx_hkl_checksum              28357