INDOLPhosphole and INDOLPhos Palladium−Allyl Complexes in Asymmetric Allylic Alkylations
Wassenaar, Jeroen; van Zutphen, Steven; Mora, Guilhem; Le Floch, Pascal; Siegler, Maxime A.; Spek, Anthony L.; Reek, Joost N. H.; Organometallics 28 (2009) 2724–; doi:10.1021/om801204a

data_4069018
_publ_section_title
;
 INDOLPhosphole and INDOLPhos Palladium&#x2212;Allyl Complexes in
 Asymmetric Allylic Alkylations
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2724
_journal_paper_doi               10.1021/om801204a
_journal_volume                  28
_journal_year                    2009
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C38 H32 N O2 P2 Pd, F6 P, 0.5 (C H2 Cl2)'
_chemical_formula_sum            'C38.5 H33 Cl F6 N O2 P3 Pd'
_chemical_formula_weight         890.42
_chemical_name_systematic
; 
 ? 
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.715(1)
_cell_angle_beta                 92.600(1)
_cell_angle_gamma                90.599(2)
_cell_formula_units_Z            4
_cell_length_a                   15.6617(4)
_cell_length_b                   15.8329(4)
_cell_length_c                   16.2065(5)
_cell_measurement_reflns_used    47978
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.68
_cell_volume                     3967.63(19)
_computing_cell_refinement       'PEAKREF (Schreurs, 2005)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            90387
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1989
_refine_ls_number_reflns         36340
_refine_ls_number_restraints     421
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0419P)^2^+1.2169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                32022
_reflns_number_total             36340
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om801204a_si_001.cif
_cod_data_source_block           5
_cod_database_code               4069018