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_4087863
_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_absolute_configuration ad
_chemical_formula_moiety         'Mo12 O40 P, 3(C20 H18 Au N P)'
_chemical_formula_sum            'C60 H54 Au3 Mo12 N3 O40 P4'
_chemical_formula_weight         3323.12
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   19.2972(9)
_cell_length_b                   19.2972(9)
_cell_length_c                   19.2127(5)
_cell_measurement_reflns_used    5138
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     6195.9(4)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9098
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         1.615
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    7.225
_exptl_absorpt_correction_T_max  0.37678
_exptl_absorpt_correction_T_min  0.34360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.672
_exptl_crystal_description       prism
_exptl_crystal_F_000             4668
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.429
_refine_diff_density_min         -2.068
_refine_diff_density_rms         0.502
_refine_ls_abs_structure_details
;
 Flack x determined using 1872 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5501
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0668P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.742
_reflns_Friedel_fraction_full    0.814
_reflns_Friedel_fraction_max     0.742
_reflns_number_gt                4767
_reflns_number_total             5501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00656_si_005.cif
_cod_data_source_block           compound_3a
_cod_original_cell_volume        6195.9(6)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4087863
_shelxl_version_number           2013-4
_shelx_res_checksum              50270
_shelx_hkl_checksum              88671