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_4087862
_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         'O40 P W12, 3(C20 H18 Au N P)'
_chemical_formula_sum            'C60 H54 Au3 N3 O40 P4 W12'
_chemical_formula_weight         4378.04
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                120.000(5)
_cell_formula_units_Z            3
_cell_length_a                   19.364(5)
_cell_length_b                   19.364(5)
_cell_length_c                   19.277(5)
_cell_measurement_reflns_used    5909
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.65
_cell_volume                     6260(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11732
_diffrn_reflns_point_group_measured_fraction_full 0.771
_diffrn_reflns_point_group_measured_fraction_max 0.695
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.984
_diffrn_reflns_theta_min         2.103
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    21.874
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.484
_exptl_crystal_description       prism
_exptl_crystal_F_000             5820
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.571
_refine_diff_density_min         -1.909
_refine_diff_density_rms         0.196
_refine_ls_abs_structure_details
;
 Flack x determined using 1491 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.013(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5638
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0215
_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^)+(0.0053P)^2^+3.6723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0421
_reflns_Friedel_coverage         0.391
_reflns_Friedel_fraction_full    0.541
_reflns_Friedel_fraction_max     0.390
_reflns_number_gt                5387
_reflns_number_total             5638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00656_si_004.cif
_cod_data_source_block           compound_2a
_cod_original_cell_volume        6260(4)
_cod_database_code               4087862
_shelxl_version_number           2013-4
_shelx_res_checksum              56393
_shelx_hkl_checksum              37798