Bimetallic Cluster Complexes: The Synthesis, Structures, and Bonding of Ruthenium Carbonyl Cluster Complexes Containing Palladium and Platinum with the Bulky Tri-tert-butyl-phosphine Ligand
Richard D. Adams; Burjor Captain; Wei Fu; Michael B. Hall; Josiah Manson; Mark D. Smith; Charles Edwin Webster; Journal of the American Chemical Society 126 (2004) 5253–5267; doi:10.1021/ja039541p

data_4112482
_publ_section_title
;
 Bimetallic Cluster Complexes: The Synthesis, Structures, and Bonding of
 Ruthenium Carbonyl Cluster Complexes Containing Palladium and Platinum
 with the Bulky Tri-tert-butyl-phosphine Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5253
_journal_page_last               5267
_journal_paper_doi               10.1021/ja039541p
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C33 H33 O14 P Pd Ru6'
_chemical_formula_weight         1397.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.464(2)
_cell_angle_beta                 88.967(2)
_cell_angle_gamma                81.998(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9793(9)
_cell_length_b                   13.7655(14)
_cell_length_c                   17.1762(18)
_cell_measurement_reflns_used    2894
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      2.43
_cell_volume                     2052.1(4)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.619 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_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  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18309
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    2.677
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.261
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                6010
_reflns_number_total             8046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja039541psi20031119_092531.cif
_cod_data_source_block           bcru6bzs
_cod_database_code               4112482