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_7101414
_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         'C108 H88 Cl4 O12 P4 Pd2'
_chemical_formula_sum            'C108 H88 Cl4 O12 P4 Pd2'
_chemical_formula_weight         2056.26
_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                 93.354(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.6433(17)
_cell_length_b                   19.522(3)
_cell_length_c                   18.184(2)
_cell_measurement_reflns_used    2544
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.341
_cell_measurement_theta_min      2.436
_cell_volume                     5543.7(12)
_computing_cell_refinement       'Bruker SMART V5.054 (Bruker, 1998)'
_computing_data_collection       'Bruker SMART V5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT V6.0 (Bruker, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V6.1 (Bruker AXS, 2000)'
_computing_publication_material  'Bruker SHELXTL V6.1 (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.876
_diffrn_measured_fraction_theta_max 0.876
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_sigmaI/netI    0.1275
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21718
_diffrn_reflns_theta_full        70.03
_diffrn_reflns_theta_max         70.03
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.484
_exptl_absorpt_correction_T_max  0.450000
_exptl_absorpt_correction_T_min  0.142495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.296
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1178
_refine_ls_number_reflns         14271
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                11754
_reflns_number_total             14271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b609704a.txt
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7101414