Synthesis, Stereochemistry, and Solution Dynamics of Heterobimetallic Complexes with Metals Connected by Dithioxamides in κ-S,S‘ κ-N,N‘ Binucleation Mode. The Molecular Structure of [2-(Diphenylphosphino)pyridine-Pt-Cl-(μ-N,N‘- dibenzyldithioxbisamidato-κ-S,S‘-Pt-κ-N,N‘-Pd)(η3-allyl)Pd]
Lanza, Santo; Bruno, Giuseppe; Nicolò, Francesco; Rotondo, Archimede; Scopelliti, Rosario; Rotondo, Enrico; Organometallics 19 (2000) 2462–; doi:10.1021/om991008o

data_4077722
_publ_contact_author
;
      Prof. Santo Lanza
      Dip. di Chimica Inorganica, Chimica Analitica e Chimica Fisica
      Universita' di Messina
      98166 Vill. Sant'Agata 
      Messina
      Italy
;
_publ_section_title
;
 Synthesis, Stereochemistry, and Solution Dynamics of Heterobimetallic
 Complexes with Metals Connected by Dithioxamides in \k-S,S&#x2018;
 \k-N,N&#x2018; Binucleation Mode. The Molecular Structure of
 [2-(Diphenylphosphino)pyridine-Pt-Cl-(\m-N,N&#x2018;-
 dibenzyldithioxbisamidato-\k-S,S&#x2018;-Pt-\k-N,N&#x2018;-Pd)(\h3-allyl)Pd]
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2462
_journal_paper_doi               10.1021/om991008o
_journal_volume                  19
_journal_year                    2000
_chemical_compound_source        'chemical synthesys'
_chemical_formula_moiety         'C36 H33 Cl N3 O2 P Pd Pt S2, C H Cl3'
_chemical_formula_sum            'C37 H34 Cl4 N3 O2 P Pd Pt S2'
_chemical_formula_weight         1091.05
_chemical_name_systematic
; 
2-(Diphenylphosphinopyridine)ChloroPlatinum(II)
(\m-N,N'Dibenzyldithioxamidato \k-S,S Pt - \k-N,N Pd)(\h^3^-Allyl)-
Palladium(II).

;
_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                111.44(2)
_cell_angle_beta                 108.482(19)
_cell_angle_gamma                91.43(2)
_cell_formula_units_Z            2
_cell_length_a                   11.648(3)
_cell_length_b                   13.542(4)
_cell_length_c                   15.046(4)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      15.6
_cell_measurement_theta_min      5.4
_cell_volume                     2068.3(11)
_computing_cell_refinement       P3/V
_computing_data_collection       'P3/V (Siemens,1989)'
_computing_data_reduction        'SHELXTL PLUS (Sheldrick, 1990)'
_computing_molecular_graphics    'XPW (Siemens, 1996)'
_computing_publication_material  'PARST97 (Nardelli, 1995) and SHELXL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w-2\q
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.1356
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8211
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         25.55
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.247
_exptl_absorpt_correction_T_max  0.7847
_exptl_absorpt_correction_T_min  0.5153
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scan method among Kopfmann & Huber, 1968
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       0.0019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.791
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7752
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      0.783
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.177
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1335
_reflns_number_gt                3987
_reflns_number_total             7752
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om991008o.cif
_cod_data_source_block           global
_cod_original_cell_volume        2068.3(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077722