Chiral triaryl phosphite-based palladacycles and platinacycles: synthesis and application to asymmetric Lewis acid catalysis
Bedford, Robin B.; Dumycz, Helena; Haddow, Mairi F.; Pilarski, Lukasz T.; Orpen, A. Guy; Pringle, Paul G.; Wingad, Richard L.; Dalton Transactions  (2009) 7796–7804; doi:10.1039/b907333g

data_7002228
_publ_section_title
;
 Chiral triaryl phosphite-based palladacycles and platinacycles:
 synthesis and application to asymmetric Lewis acid catalysis
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              7796
_journal_page_last               7804
_journal_paper_doi               10.1039/b907333g
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C55 H58 Cl N2 O3 P Pd, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C56.5 H61 Cl4 N2 O3 P Pd'
_chemical_formula_weight         1095.24
_chemical_name_systematic
;
?
;
_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                   14.495(3)
_cell_length_b                   16.679(3)
_cell_length_c                   21.684(4)
_cell_measurement_reflns_used    25839
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.481
_cell_measurement_theta_min      2.241
_cell_volume                     5242.4(17)
_computing_cell_refinement       'Bruker SMART V5.628 (Bruker, 2005)'
_computing_data_collection       'Bruker SMART V5.628 (Bruker, 2005)'
_computing_data_reduction        'Bruker SAINT V6.41A (Bruker, 2002)'
_computing_molecular_graphics    'Bruker SHELXTL V6.14 (Bruker AXS, 2003)'
_computing_publication_material  'Bruker SHELXTL V6.14 (Bruker AXS, 2003)'
_computing_structure_refinement  'SHELXL V6.12 (Bruker 2001)'
_computing_structure_solution    'SHELXS V6.12 (Bruker 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60588
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.900000
_exptl_absorpt_correction_T_min  0.789671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Bruker AXS 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.574
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, based on 5426 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.027(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         12029
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0534P)^2^+3.5790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                11636
_reflns_number_total             12029
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907333g.txt
_cod_data_source_block           ltp1b68sad
_cod_original_cell_volume        5242.4(18)
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'C56.50 H61 Cl4 N2 O3 P Pd'
_cod_database_code               7002228