Reactivity of (Ferrocenylmethyl)phosphine toward Palladium and Platinum Chlorides. X-ray Structure of [Pd(PH2CH2Fc)Cl(μ-PHCH2Fc)]4(Fc = Ferrocenyl), a Unique Complex Containing a Pd4P4Cycle
Dell'Anna, Maria Michela; Englert, Ulli; Latronico, Mario; Luis, Pablo Lorenzo; Mastrorilli, Piero; Papa, Daniela Giardina; Nobile, Cosimo Francesco; Peruzzini, Maurizio; Inorganic Chemistry 45 (2006) 6892–6900; doi:10.1021/ic060311w

data_4332388
_publ_section_title
;
 Reactivity of (Ferrocenylmethyl)phosphine toward Palladium and Platinum
 Chlorides. X-ray Structure of [Pd(PH2CH2Fc)Cl(\m-PHCH2Fc)]4(Fc =
 Ferrocenyl), a Unique Complex Containing a Pd4P4Cycle
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6892
_journal_page_last               6900
_journal_paper_doi               10.1021/ic060311w
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C100 H124 Cl4 Fe8 O3 P8 Pd4'
_chemical_formula_weight         2635.95
_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                107.120(12)
_cell_angle_beta                 96.344(13)
_cell_angle_gamma                117.087(15)
_cell_formula_units_Z            2
_cell_length_a                   17.607(7)
_cell_length_b                   17.944(7)
_cell_length_c                   18.792(7)
_cell_measurement_reflns_used    2620
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.23
_cell_volume                     4839(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full .998
_diffrn_measured_fraction_theta_max .998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.1238
_diffrn_reflns_av_sigmaI/netI    0.1573
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52647
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    2.177
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_platon_squeeze_details
; a large void around an inversion center (.5, .0, .5) in 
space group P-1 (no. 2) was encountered; attempts to model the 
electron density to the solvents of crystallization, thf,
gave unsatisfactory results.
In agreement with the solvent of crystallization, the volume 
of 600 A3 and the electron count of 240, this large void 
contains six molecules of tetrahydrofuran, C4H8O. Derived 
crystal data such as density, formula weight, and linear 
absorption coefficient have been corrected for the presence of 
these moieties.
Lit: P. van der Sluis & A.L. Spek (1990). Acta Cryst. A46, 194-201 
;
_refine_diff_density_max         1.973
_refine_diff_density_min         -1.498
_refine_diff_density_rms         .243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         16980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.1669
_refine_ls_R_factor_gt           0.1246
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+116.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2544
_refine_ls_wR_factor_ref         0.2763
_reflns_number_gt                12091
_reflns_number_total             16980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060311wsup1.cif
_cod_data_source_block           pm17
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               4332388