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_4076303
_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         'C69 H20 Pd1 S2'
_chemical_formula_structural     'C69 H20 Pd1 S2'
_chemical_formula_sum            'C69 H20 Pd S2'
_chemical_formula_weight         1019.37
_chemical_name_systematic
;
 PdC60Me5allyl
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2002-11-19T21:48:55-00:00
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   17.775(5)
_cell_length_b                   12.451(5)
_cell_length_c                   17.726(5)
_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                     3923(2)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.868
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3322
_diffrn_reflns_theta_full        25.61
_diffrn_reflns_theta_max         25.61
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.751
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(5)
_refine_ls_extinction_coef       0.0124(17)
_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   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         3322
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0683
_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^)+(0.1701P)^2^+3.9202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.1924
_reflns_number_gt                3225
_reflns_number_total             3322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0499153si20040202_081546.cif
_cod_data_source_block           7a
_cod_database_code               4076303