Chelate-Size Effects on the Structures, Chemical Behavior, Properties, and Catalytic Activity of the New Palladium(II)−Allyl Complexes [Pd(η3-1-R1-C3H4){FcCHN-CH2-(CH2)n-NMe2}][PF6] {Fc = (η5-C5H5)Fe(η5-C5H4),n= 2 or 1, and R1= H or Ph}
Pérez, Sonia; López, Concepción; Bosque, Ramon; Solans, Xavier; Font-Bardía, Mercè; Roig, Anna; Molins, Elies; van Leeuwen, Piet W. N. M.; van Strijdonck, Gino P. F.; Freixa, Zoraida; Organometallics 27 (2008) 4288–; doi:10.1021/om7012452

data_4071088
_publ_section_title
;
 Chelate-Size Effects on the Structures, Chemical Behavior, Properties,
 and Catalytic Activity of the New Palladium(II)&#x2212;Allyl Complexes
 [Pd(\h3-1-R1-C3H4){FcCH&#xE5FB;N-CH2-(CH2)n-NMe2}][PF6] {Fc =
 (\h5-C5H5)Fe(\h5-C5H4),n= 2 or 1, and R1= H or Ph}
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4288
_journal_paper_doi               10.1021/om7012452
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C19 H27 Fe N2 Pd, F6 P'
_chemical_formula_sum            'C19 H27 F6 Fe N2 P Pd'
_chemical_formula_weight         590.65
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7170(10)
_cell_length_b                   14.2960(10)
_cell_length_c                   16.1650(10)
_cell_measurement_reflns_used    13504
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     2245.5(3)
_computing_cell_refinement       AUTOMAR
_computing_data_collection       MARXDS
_computing_data_reduction        MARSCALE
_computing_molecular_graphics    'ORTEP (Brueggermann and Smith, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.885
_diffrn_measured_fraction_theta_max 0.766
_diffrn_measurement_device_type  'MAR345 with image plate detector'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15155
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.61
_diffrn_reflns_theta_min         2.10
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.575
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.976
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.019(4)
_refine_ls_extinction_coef       0.042(4)
_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   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         3223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+2.0199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1538
_reflns_number_gt                2959
_reflns_number_total             3223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7012452_si_003.cif
_cod_data_source_block           chgm12
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4071088