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_7002229
_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 Pt2'
_chemical_formula_sum            'C68 H64 Cl2 O6 P2 Pt2'
_chemical_formula_weight         1500.21
_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                 108.246(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.724(3)
_cell_length_b                   10.2340(16)
_cell_length_c                   17.561(3)
_cell_measurement_reflns_used    143
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.33
_cell_volume                     3025.2(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9873
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    4.812
_exptl_absorpt_correction_T_max  0.618
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.05'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.165
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, based on 3084 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.009(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6748
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0393P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                5712
_reflns_number_total             6748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907333g.txt
_cod_data_source_block           choclatsad
_cod_original_sg_symbol_Hall     C2y
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7002229