Chiral palladium bis(phosphite) PCP-pincer complexes via ligand C‒H activation
Baber, R. Angharad; Bedford, Robin B.; Betham, Michael; Blake, Michael E.; Coles, Simon J.; Haddow, Mairi F.; Hursthouse, Michael B.; Orpen, A. Guy; Pilarski, Lukasz T.; Pringle, Paul G.; Wingada, Richard L.; Chemical Communications (Cambridge, United Kingdom)  (2006) 3880–3882; doi:10.1039/b609704a

data_7101413
_publ_section_title
;
 Chiral palladium bis(phosphite) PCP-pincer complexes via ligand C--H
 activation
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   37
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              3880
_journal_page_last               3882
_journal_paper_doi               10.1039/b609704a
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C46 H27 Cl O6 P2 Pd, 3(C H Cl3)'
_chemical_formula_sum            'C49 H30 Cl10 O6 P2 Pd'
_chemical_formula_weight         1237.57
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.57(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.425(2)
_cell_length_b                   9.2502(19)
_cell_length_c                   25.909(5)
_cell_measurement_reflns_used    1383
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.341
_cell_measurement_theta_min      2.339
_cell_volume                     2486.8(9)
_computing_cell_refinement       'Bruker SMART V5.625 (Bruker, 2001)'
_computing_data_collection       'Bruker SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT V6.28 (Bruker, 2001)'
_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      293(2)
_diffrn_detector_area_resol_mean 8.5
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0579
_diffrn_reflns_av_sigmaI/netI    0.1234
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            17578
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  0.950000
_exptl_absorpt_correction_T_min  0.657985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Bruker AXS, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         10930
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                8341
_reflns_number_total             10930
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b609704a.txt
_cod_original_sg_symbol_Hall     P2yb
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7101413