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_4077974
_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            'C131.5 H113 O14.5 P6 Pd9 Tl'
_chemical_formula_weight         3273.01
_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                88.8100(10)
_cell_angle_beta                 88.7240(10)
_cell_angle_gamma                80.6750(10)
_cell_formula_units_Z            4
_cell_length_a                   17.5842(8)
_cell_length_b                   26.4171(13)
_cell_length_c                   26.6018(13)
_cell_measurement_temperature    100(2)
_cell_volume                     12189.0(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.956
_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  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            113530
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         0.77
_exptl_absorpt_coefficient_mu    2.752
_exptl_absorpt_correction_T_max  0.6830
_exptl_absorpt_correction_T_min  0.3983
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black-red
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'block crystal'
_exptl_crystal_F_000             6412
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         6.914
_refine_diff_density_min         -2.752
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2917
_refine_ls_number_reflns         58013
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0610P)^2^+211.7120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1653
_refine_ls_wR_factor_ref         0.1771
_reflns_number_gt                45047
_reflns_number_total             58013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201150x_si_002.cif
_cod_data_source_block           dahl313
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C131.50 H113 O14.50 P6 Pd9 Tl'
_cod_database_code               4077974