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_7002230
_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         'C68 H64 Cl2 O6 P2 Pd2'
_chemical_formula_sum            'C68 H64 Cl2 O6 P2 Pd2'
_chemical_formula_weight         1322.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 108.220(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.694(4)
_cell_length_b                   10.290(2)
_cell_length_c                   17.527(4)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.32
_cell_volume                     3031.2(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.1106
_diffrn_reflns_av_sigmaI/netI    0.2131
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9750
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.05'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.871
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, based on 1944 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5548
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1599
_refine_ls_R_factor_gt           0.0671
_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^)+(0.0416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1355
_reflns_number_gt                3085
_reflns_number_total             5548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907333g.txt
_cod_data_source_block           berwicksad
_cod_original_cell_volume        3031.0(10)
_cod_original_sg_symbol_Hall     C2y
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7002230