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_4342913
_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         'C6 H18 Cl2 P2 Pd, C H Cl3'
_chemical_formula_sum            'C7 H19 Cl5 P2 Pd'
_chemical_formula_weight         448.81
_chemical_name_systematic
; 
 cis-Dichloro- bis(trimetylphosphine)palladium (II)  
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.3220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.1667(7)
_cell_length_b                   28.1052(19)
_cell_length_c                   11.6394(8)
_cell_measurement_temperature    100(2)
_cell_volume                     3325.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30644
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         0.72
_exptl_absorpt_coefficient_mu    2.084
_exptl_absorpt_correction_T_max  0.6807
_exptl_absorpt_correction_T_min  0.5209
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SHELXTL (version 6.14 (2000-2003)) program library 
;
_exptl_crystal_colour            'light-yellow to colorless'
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.328
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         8169
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+9.2328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                7762
_reflns_number_total             8169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00208_si_002.cif
_cod_data_source_block           dahl335
_cod_depositor_comments
'Adding full bibliography for 4342911--4342913.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4342913