Investigation of Steric and Electronic Features of 3-Iminophosphine-Based Palladium Catalysts for Intermolecular Hydroamination
Zingales, Nicholas C.; Shaffer, Andrew R.; Schmidt, Joseph A. R.; Organometallics 32 (2013) 578–; doi:10.1021/om301102w

data_4079961
_publ_section_title
;
 Investigation of Steric and Electronic Features of 3-Iminophosphine-Based
 Palladium Catalysts for Intermolecular Hydroamination
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              578
_journal_paper_doi               10.1021/om301102w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C23 H41 F3 N O3 P Pd S'
_chemical_formula_weight         606.00
_chemical_name_common            8Pd
_chemical_name_systematic
; 
 ? 
;
_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                73.83(3)
_cell_angle_beta                 79.74(3)
_cell_angle_gamma                84.99(3)
_cell_formula_units_Z            2
_cell_length_a                   10.315(2)
_cell_length_b                   10.453(2)
_cell_length_c                   13.040(3)
_cell_measurement_reflns_used    5201
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      1.65
_cell_volume                     1327.7(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30580
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6387
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.809
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+24.6159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.1923
_reflns_number_gt                4754
_reflns_number_total             5201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301102w_si_003.cif
_cod_data_source_block           8Pd
_cod_original_cell_volume        1327.8(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4079961