High-Yield Synthesis of PPh3-Ligated Decanuclear Tl‒Pd Cluster, Pd9[Tl(acac)](CO)9(PPh3)6: Comparative Analysis of Tl(I)‒Pd(0) Bonding Connectivities with Known Tl‒Pd Clusters and Resulting Insight Concerning Their Dissimilar Dynamic Solution Behavior
Mednikov, Evgueni G.; Vo, Nicky; Fry, Charles G.; Dahl, Lawrence F.; Organometallics 31 (2012) 2878–; doi:10.1021/om201150x

data_4077975
_publ_section_title
;
 High-Yield Synthesis of PPh3-Ligated Decanuclear Tl--Pd Cluster,
 Pd9[Tl(acac)](CO)9(PPh3)6: Comparative Analysis of Tl(I)--Pd(0) Bonding
 Connectivities with Known Tl--Pd Clusters and Resulting Insight
 Concerning Their Dissimilar Dynamic Solution Behavior
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2878
_journal_paper_doi               10.1021/om201150x
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C123.2 H99.4 O11.3 P6 Pd9 Tl'
_chemical_formula_weight         3108.42
_chemical_name_common
;
palladium-thallium carbonylphosphine acetylacetonate
;
_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                107.682(2)
_cell_angle_beta                 92.176(2)
_cell_angle_gamma                99.572(2)
_cell_formula_units_Z            4
_cell_length_a                   16.6815(5)
_cell_length_b                   23.9936(7)
_cell_length_c                   30.3230(9)
_cell_measurement_reflns_used    9025
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.2729
_cell_measurement_theta_min      2.8521
_cell_volume                     11351.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker Apex2 diffractometer'
_diffrn_measurement_method       'w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            180753
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         72.27
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        '< 1'
_exptl_absorpt_coefficient_mu    15.154
_exptl_absorpt_correction_T_max  0.5754
_exptl_absorpt_correction_T_min  0.1914
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate crystal'
_exptl_crystal_F_000             6056
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.521
_refine_diff_density_min         -2.029
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2127
_refine_ls_number_reflns         42046
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.630
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.002
_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          0.1331
_refine_ls_wR_factor_ref         0.1506
_reflns_number_gt                32669
_reflns_number_total             42046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201150x_si_003.cif
_cod_data_source_block           dahl391
_cod_original_formula_sum        'C123.20 H99.40 O11.30 P6 Pd9 Tl'
_cod_database_code               4077975