Fast and Reversible Intramolecular Cleavage of an Au−C Bond in the Spiked-Triangular Metal Complexes [Fe3Au(μ4,η2-C⋮CtBu)(CO)9(PR3)] (R = Ph,iPr)
Delgado, Esther; Donnadieu, Bruno; García, M. Esther; García, Silvia; Ruiz, Miguel A.; Zamora, Félix; Organometallics 21 (2002) 780–; doi:10.1021/om010980b

data_4076720
_publ_contact_author             'Dr Esther Delgado'
_publ_section_title
;
 Fast and Reversible Intramolecular Cleavage of an Au&#x2212;C Bond in the
 Spiked-Triangular Metal Complexes
 [Fe3Au(\m4,\h2-C&#x22EE;CtBu)(CO)9(PR3)] (R = Ph,iPr)
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              780
_journal_paper_doi               10.1021/om010980b
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C33 H24 Au Fe3 O9 P'
_chemical_formula_weight         960.01
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 98.531(5)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   15.087(5)
_cell_length_b                   9.997(5)
_cell_length_c                   23.272(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.2
_cell_volume                     3471(2)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19848
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    5.539
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.05
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         4969
_refine_ls_number_restraints     382
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          1.206
_refine_ls_shift/su_mean         0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+3.6409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                3856
_reflns_number_total             4969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010980b.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4076720