Changes in Coordination of Sterically Demanding Hybrid Imidazolylphosphine Ligands on Pd(0) and Pd(II)
Douglas B. Grotjahn; Yi Gong; Lev Zakharov; James A. Golen; Arnold L. Rheingold; Journal of the American Chemical Society 128 (2006) 438–453; doi:10.1021/ja054779u

data_4110359
_publ_section_title
;
 Changes in Coordination of Sterically Demanding Hybrid
 Imidazolylphosphine Ligands on Pd(0) and Pd(II)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              438
_journal_page_last               453
_journal_paper_doi               10.1021/ja054779u
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C18 H28 I N2 P Pd'
_chemical_formula_weight         536.69
_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                90.00
_cell_angle_beta                 102.8490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9008(5)
_cell_length_b                   16.7186(9)
_cell_length_c                   12.9150(7)
_cell_measurement_reflns_used    9333
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.44
_cell_volume                     2084.26(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      147(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12908
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    2.450
_exptl_absorpt_correction_T_max  0.7917
_exptl_absorpt_correction_T_min  0.3739
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0340P)^2^+0.7593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                4361
_reflns_number_total             4808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054779usi20050716_085059.cif
_cod_data_source_block           grot71
_cod_database_code               4110359