Nanosized {Pd4(μ4-C)}Pd32(CO)28(PMe3)14 Containing Tetrahedrally Deformed Pd4 Cage with Encapsulated Carbide Atom: Formal Substitution of Geometrically Analogous Interior Au4 Entity in Isostructural Au4Pd32(CO)28(PMe3)14 by Electronically Equivalent Pd4(μ4-C) and Computational/Catalytic Implications.
Mednikov, Evgueni G.; Ivanov, Sergei A.; Dahl, Lawrence F.; Inorganic chemistry 54 (2015) 6157–6168; doi:10.1021/acs.inorgchem.5b00208

data_4342912
_publ_section_title
;
 Nanosized {Pd4(\m4-C)}Pd32(CO)28(PMe3)14 Containing Tetrahedrally
 Deformed Pd4 Cage with Encapsulated Carbide Atom: Formal Substitution of
 Geometrically Analogous Interior Au4 Entity in Isostructural
 Au4Pd32(CO)28(PMe3)14 by Electronically Equivalent Pd4(\m4-C) and
 Computational/Catalytic Implications.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6157
_journal_page_last               6168
_journal_paper_doi               10.1021/acs.inorgchem.5b00208
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C71 H126 O28 P14 Pd36, C3 H3 Cl9'
_chemical_formula_sum            'C74 H129 Cl9 O28 P14 Pd36'
_chemical_formula_weight         6049.80
_chemical_name_common
;
 Palladium Carbonyl Phosphine Carbido Cluster 
;
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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                87.771(2)
_cell_angle_beta                 81.1850(10)
_cell_angle_gamma                80.0530(10)
_cell_formula_units_Z            2
_cell_length_a                   16.0975(16)
_cell_length_b                   17.7114(17)
_cell_length_c                   25.768(3)
_cell_measurement_temperature    100(2)
_cell_volume                     7150.2(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'SMART CCD 1000 area detector difractometer'
_diffrn_measurement_method       'w 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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            90528
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    4.773
_exptl_absorpt_correction_T_max  0.7963
_exptl_absorpt_correction_T_min  0.3700
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             5632
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.878
_refine_diff_density_min         -2.705
_refine_diff_density_rms         0.389
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.329
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1438
_refine_ls_number_reflns         34207
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.329
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1956
_refine_ls_wR_factor_ref         0.2073
_reflns_number_gt                25478
_reflns_number_total             34207
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00208_si_002.cif
_cod_data_source_block           dahl336
_cod_depositor_comments
'Adding full bibliography for 4342911--4342913.cif.'
_cod_original_cell_volume        7150.2(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4342912