Palladium-Arene Interactions in Catalytic Intermediates: An Experimental and Theoretical Investigation of the Soft Rearrangement between η1 and η2 Coordination Modes
Marta Catellani; Carlo Mealli; Elena Motti; Paola Paoli; Enrique Perez-Carreño; Paul S. Pregosin; Journal of the American Chemical Society 124 (2002) 4336–4346; doi:10.1021/ja016587e

data_4114750
_publ_contact_author
;
Dr. Carlo Mealli
Istituto per lo Studio della Stereochimica ed Energetica
dei Composti di Coordinazione CNR
Via J. Nardi 39
I-50132 Firenze
;
_publ_contact_author_email       mealli@fi.cnr.it
_publ_section_title
;
 Palladium-Arene Interactions in Catalytic Intermediates: An Experimental
 and Theoretical Investigation of the Soft Rearrangement between \h1 and
 \h2 Coordination Modes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4336
_journal_page_last               4346
_journal_paper_doi               10.1021/ja016587e
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety
'(C15 H19 1-)2, (Cl 1-)2, (Pd 2+)2, (C H2 Cl2)'
_chemical_formula_sum            'C31 H40 Cl4 Pd2'
_chemical_formula_weight         767.23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 115.962(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   11.785(5)
_cell_length_b                   21.824(5)
_cell_length_c                   12.937(5)
_cell_measurement_temperature    100
_cell_volume                     2991.6(19)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP (Johnson)'
_computing_publication_material  'PARST97 (Nardelli 1983)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_radiation_monochromator  'Gobel mirrors'
_diffrn_radiation_source         'Siemens Cu rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4000
_diffrn_reflns_theta_full        58.82
_diffrn_reflns_theta_max         58.82
_diffrn_reflns_theta_min         4.05
_exptl_absorpt_coefficient_mu    13.127
_exptl_absorpt_correction_T_max  0.4198
_exptl_absorpt_correction_T_min  0.3018
_exptl_absorpt_process_details   XABS2
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.714
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.210
_refine_ls_extinction_coef       0.00018(5)
_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   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         4000
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+63.6490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                3221
_reflns_number_total             4000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja016587e_s1.cif
_cod_data_source_block           '[(C15H19)PdCl]2.CH2Cl2'
_cod_original_cell_volume        2991.6(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4114750