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_4110365
_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            'C37 H66 F3 N5 O3 P Pd S'
_chemical_formula_weight         855.38
_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 91.5240(10)
_cell_angle_gamma                105.1180(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2846(9)
_cell_length_b                   13.6817(10)
_cell_length_c                   13.7439(9)
_cell_measurement_reflns_used    7128
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.61
_cell_volume                     2254.2(3)
_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      213(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15104
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.510
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         8765
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                7503
_reflns_number_total             8765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054779usi20050716_085222.cif
_cod_data_source_block           grot121
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