First high-nuclearity thallium–palladium carbonyl phosphine cluster, [Tl~2~Pd~12~(CO)~9~(PEt~3~)~9~]^2+^, and its initial mistaken identity as the unknown Au~2~Pd~12~ analogue: structure-to-synthesis approach concerning its formation
Ivanov, Sergei A.; Nichiporuk, Rita V.; Mednikov, Eugeny G.; Dahl, Lawrence F.; Journal of the Chemical Society, Dalton Transactions  (2002) 4116–4127; doi:10.1039/b204276m

data_7011813
_publ_section_title
;
 First high-nuclearity thallium--palladium carbonyl phosphine cluster,
 [Tl~2~Pd~12~(CO)~9~(PEt~3~)~9~]^2+^, and its initial mistaken identity as
 the unknown Au~2~Pd~12~ analogue: structure-to-synthesis approach concerning
 its formation
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4116
_journal_page_last               4127
_journal_paper_doi               10.1039/b204276m
_journal_year                    2002
_chemical_formula_sum            'C63 H135 F12 O9 P11 Pd12 Tl2'
_chemical_formula_weight         3290.92
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.3656(16)
_cell_length_b                   24.4157(14)
_cell_length_c                   29.9053(17)
_cell_measurement_reflns_used    7452
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      1.67
_cell_volume                     19981(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            150698
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count N/A
_diffrn_standards_interval_time  N/A
_diffrn_standards_number         N/A
_exptl_absorpt_coefficient_mu    5.555
_exptl_absorpt_correction_T_max  0.6971
_exptl_absorpt_correction_T_min  0.2865
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Empirical with SADABS (Blessing, 1995)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.188
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             12576
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.072
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         18993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0635P)^2^+203.6154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                14852
_reflns_number_total             18993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204276m.txt
_cod_data_source_block           tl2pd12
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7011813