Nickel, Palladium, and Platinum Complexes of η5-Cyclopentadienide C60R5Ligands. Kinetic and Thermodynamic Stabilization Effects of the C60Ph5Ligand
Kuninobu, Yoichiro; Matsuo, Yutaka; Toganoh, Motoki; Sawamura, Masaya; Nakamura, Eiichi; Organometallics 23 (2004) 3259–; doi:10.1021/om0499153

data_4076306
_publ_contact_author             'Nakamura, E.'
_publ_section_title
;
 Nickel, Palladium, and Platinum Complexes of \h5-Cyclopentadienide
 C60R5Ligands. Kinetic and Thermodynamic Stabilization Effects of the
 C60Ph5Ligand
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3259
_journal_paper_doi               10.1021/om0499153
_journal_volume                  23
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C90 H30 Pd1'
_chemical_formula_structural     'C90 H30 Pd1'
_chemical_formula_sum            'C94.25 H32 Pd S0.5'
_chemical_formula_weight         1286.63
_chemical_name_systematic
;
 PdC60Ph5metallyl
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2002-11-21T01:20:40-00:00
_cell_angle_alpha                65.206(3)
_cell_angle_beta                 80.338(3)
_cell_angle_gamma                78.855(4)
_cell_formula_units_Z            4
_cell_length_a                   13.4150(11)
_cell_length_b                   21.3700(12)
_cell_length_c                   21.1590(16)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     5377.1(7)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18245
_diffrn_reflns_theta_full        25.82
_diffrn_reflns_theta_max         25.82
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2606
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.782
_refine_diff_density_min         -1.794
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.0154(10)
_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   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1727
_refine_ls_number_reflns         18245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1777P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2118
_refine_ls_wR_factor_ref         0.2541
_reflns_number_gt                12391
_reflns_number_total             18245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0499153si20040202_081709.cif
_cod_data_source_block           8b
_cod_original_formula_sum        'C94.25 H32 Pd S0.50'
_cod_database_code               4076306