Cooperative Effects of Electron Donors and Acceptors for the Stabilization of Elusive Metal Cluster Frameworks: Synthesis and Solid-State Structures of [Pt19(CO)24(μ4-AuPPh3)3]- and [Pt19(CO)24{μ4-Au2(PPh3)2}2]
Alessandro Ceriotti; Piero Macchi; Annalisa Sironi; Simona El Afefey; Matteo Daghetta; Serena Fedi; Fabrizia Fabrizi de Biani; Roberto Della Pergola; Inorganic Chemistry 52 (2013) 1960–1964; doi:10.1021/ic302282y

data_4333864
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of Bern
Freiestrasse 3
Bern, CH
;
_publ_contact_author_email       piero.macchi@dcb.unibe.ch
_publ_section_title
;
 Cooperative Effects of Electron Donors and Acceptors for the
 Stabilization of Elusive Metal Cluster Frameworks: Synthesis and
 Solid-State Structures of [Pt19(CO)24(\m4-AuPPh3)3]- and
 [Pt19(CO)24{\m4-Au2(PPh3)2}2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1960
_journal_page_last               1964
_journal_paper_doi               10.1021/ic302282y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C78 H45 Au3 O24 P3 Pt19'
_chemical_formula_weight         5756.48
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-10T14:28:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(3)
_cell_angle_beta                 91.633(3)
_cell_angle_gamma                90.000(3)
_cell_formula_units_Z            2
_cell_length_a                   15.5619(16)
_cell_length_b                   21.250(2)
_cell_length_c                   18.164(2)
_cell_measurement_temperature    173(2)
_cell_volume                     6004.2(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.12
_diffrn_reflns_av_unetI/netI     0.1375
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            64114
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    25.771
_exptl_absorpt_correction_T_max  0.0645
_exptl_absorpt_correction_T_min  0.0384
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
        Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
        for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
        p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
        A31,146-148) is used with some modification.
;
_exptl_crystal_density_diffrn    3.184
_exptl_crystal_F_000             4938
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         3.144
_refine_diff_density_min         -7.703
_refine_diff_density_rms         0.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         10538
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1619
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0944P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.223
_refine_ls_wR_factor_ref         0.2389
_reflns_number_gt                3844
_reflns_number_total             10538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302282y_si_001_1.cif
_cod_data_source_block           2
_cod_original_cell_volume        6004.0(11)
_cod_database_code               4333864