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_4066972
_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         'C31 H28 Fe N P'
_chemical_formula_sum            'C31 H28 Fe N P'
_chemical_formula_weight         501.36
_chemical_name_common            (Sp,Sc)-3
_chemical_name_systematic
; 
(Sp,Sc)-3 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4272(3)
_cell_length_b                   12.4311(5)
_cell_length_c                   23.6623(9)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.48
_cell_measurement_theta_min      2.92
_cell_volume                     2478.85(16)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'Apex 2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'SHELXTL, XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART ApexII'
_diffrn_measurement_method       '\f and \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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            32735
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.9531
_exptl_absorpt_correction_T_min  0.7503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         8244
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.3571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                7822
_reflns_number_total             8244
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om100741m_si_001.cif
_cod_data_source_block           (Sp,Sc)-3
_cod_database_code               4066972