Synthesis and Characterization of New, Chiral P−N Ligands and Their Use in Asymmetric Allylic Alkylation
Thiesen, Kurtis E.; Maitra, Kalyani; Olmstead, Marilyn M.; Attar, Saeed; Organometallics 29 (2010) 6334–; doi:10.1021/om100741m

data_4066973
_publ_section_title
;
 Synthesis and Characterization of New, Chiral P&#x2212;N Ligands and
 Their Use in Asymmetric Allylic Alkylation
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6334
_journal_paper_doi               10.1021/om100741m
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H33 Fe N P Pd, B F4'
_chemical_formula_sum            'C34 H33 B F4 Fe N P Pd'
_chemical_formula_weight         735.64
_chemical_name_common            '[Pd(C3H5)((Sp,Sc)-3]BF4,'
_chemical_name_systematic
; 
Compound 4 
;
_space_group_IT_number           1
_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                106.356(3)
_cell_angle_beta                 90.187(2)
_cell_angle_gamma                110.903(3)
_cell_formula_units_Z            1
_cell_length_a                   9.0254(2)
_cell_length_b                   9.6542(3)
_cell_length_c                   9.7700(3)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      32.6
_cell_measurement_theta_min      2.7
_cell_volume                     757.95(4)
_computing_cell_refinement       'Apex2 (Bruker, 2010)'
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'Apex2 (Bruker, 2010)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  "'SHELXTL, (Sheldrick, 1997)"
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART Apex II'
_diffrn_measurement_method       \w
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18016
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         8998
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0479P)^2^+0.2237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                8901
_reflns_number_total             8998
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om100741m_si_001.cif
_cod_data_source_block           Compound4
_cod_database_code               4066973