Synthesis, Dynamic Behavior, and Reactivity of New Unsaturated Heterotrinuclear 46 Valence Electron Complexes Polynuclear Homo- or Heterometallic Palladium(II)-Platinum(II) Pentafluorophenyl Complexes Containing Bridging Diphenylphosphido Ligands. 27. For part 26, see ref 1.
Juan Forniés; Consuelo Fortuño; Susana Ibáñez; Antonio Martín; Pilar Romero; Piero Mastrorilli; Vito Gallo; Inorganic Chemistry 50 (2011) 285–298; doi:10.1021/ic101934t

data_4324140
_publ_section_title
;
 Synthesis, Dynamic Behavior, and Reactivity of New Unsaturated
 Heterotrinuclear 46 Valence Electron Complexes Polynuclear Homo- or
 Heterometallic Palladium(II)-Platinum(II) Pentafluorophenyl Complexes
 Containing Bridging Diphenylphosphido Ligands. 27. For part 26, see ref
 1.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              285
_journal_page_last               298
_journal_paper_doi               10.1021/ic101934t
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C90.6 H79.4 F20 N O P4 Pd Pt2'
_chemical_formula_weight         2198.61
_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                85.339(2)
_cell_angle_beta                 84.915(2)
_cell_angle_gamma                76.108(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0400(4)
_cell_length_b                   15.5046(6)
_cell_length_c                   24.3942(6)
_cell_measurement_reflns_used    28674
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8873
_cell_measurement_theta_min      3.7583
_cell_volume                     4394.7(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_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      100(2)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   -1.00   53.00   0.4500   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.7123   75.0000  240.0000    0.0000    0.0000 120

  2 omega   -1.00   53.00   0.4500   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.7123   75.0000    0.0000    0.0000    0.0000 120

  3 omega  -44.00    7.75   0.4500   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.7123  -45.0000  240.0000    0.0000    0.0000 115

  4 omega    1.00   52.75   0.4500   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.7123   45.0000    0.0000    0.0000    0.0000 115

  5 omega  -52.00    2.90   0.4500   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.7123   75.0000  240.0000    0.0000    0.0000 122

  6 omega  -10.00   44.00   0.4500   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0560   75.0000    0.0000    0.0000    0.0000 120

  7 omega   38.00   81.65   0.4500   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0560 -125.0000  218.0000    0.0000    0.0000 97

  8 omega  -10.00   44.00   0.4500   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0560   75.0000  120.0000    0.0000    0.0000 120

  9 omega   -3.00   42.00   0.4500   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0560 -125.0000  218.0000    0.0000    0.0000 100

 10 omega  -50.00    4.00   0.4500   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0560  -75.0000    0.0000    0.0000    0.0000 120

 11 omega   40.00   94.00   0.4500   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0560   75.0000  120.0000    0.0000    0.0000 120

 12 omega    0.00   54.00   0.4500   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.0560  -75.0000    0.0000    0.0000    0.0000 120

;
_diffrn_measurement_device_type  'Bruker Smart'
_diffrn_measurement_method       'w scans'
_diffrn_orient_matrix_UB_11      0.0176305690
_diffrn_orient_matrix_UB_12      -0.0095164968
_diffrn_orient_matrix_UB_13      0.0272256688
_diffrn_orient_matrix_UB_21      0.0443421559
_diffrn_orient_matrix_UB_22      0.0228098320
_diffrn_orient_matrix_UB_23      -0.0067500594
_diffrn_orient_matrix_UB_31      -0.0377140860
_diffrn_orient_matrix_UB_32      0.0401058612
_diffrn_orient_matrix_UB_33      0.0081994547
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43917
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    3.539
_exptl_absorpt_correction_T_max  0.8157
_exptl_absorpt_correction_T_min  0.3114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.057
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         15556
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0474P)^2^+4.4161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                12399
_reflns_number_total             15556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101934t_si_001_6.cif
_cod_data_source_block           9
_cod_original_cell_volume        4394.7(2)
_cod_original_formula_sum        'C90.60 H79.40 F20 N O P4 Pd Pt2'
_cod_database_code               4324140