A Dicoordinate Palladium(0) Complex with an Unusual Intramolecular η1-Arene Coordination
Steven M. Reid; Robert C. Boyle; Joel T. Mague; Mark J. Fink; Journal of the American Chemical Society 125 (2003) 7816–7817; doi:10.1021/ja0361493

data_4113869
_publ_section_title
;
 A Dicoordinate Palladium(0) Complex with an Unusual Intramolecular
 \h1-Arene Coordination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7816
_journal_page_last               7817
_journal_paper_doi               10.1021/ja0361493
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C24 H31 P1 C24 H31 P1 Pd1'
_chemical_formula_sum            'C48 H62 P2 Pd'
_chemical_formula_weight         807.32
_chemical_name_systematic
; 
 Bis(dicyclohexyl(2-biphenylyl)phosphine)palladium(0)
;
_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                101.872(6)
_cell_angle_beta                 97.271(9)
_cell_angle_gamma                109.371(6)
_cell_formula_units_Z            2
_cell_length_a                   10.4353(10)
_cell_length_b                   10.5321(5)
_cell_length_c                   20.910(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2073.9(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0509
_diffrn_reflns_av_sigmaI/netI    0.1084
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6939
_diffrn_reflns_theta_full        24.08
_diffrn_reflns_theta_max         24.08
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       Column
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0331P)^2^+0.7449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                3984
_reflns_number_total             6529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0361493si20030530_011146.cif
_cod_data_source_block           mjf226
_cod_database_code               4113869