Tuning ligand structure in chiral bis(phosphite) and mixed phosphite-phosphinite PCP-palladium pincer complexes.
Bedford, Robin B.; Chang, Yu-Ning; Haddow, Mairi F.; McMullin, Claire L.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 9034–9041; doi:10.1039/c1dt10356c

data_7016385
_publ_section_title
;
 Tuning ligand structure in chiral bis(phosphite) and mixed
 phosphite-phosphinite PCP-palladium pincer complexes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9034
_journal_page_last               9041
_journal_paper_doi               10.1039/c1dt10356c
_journal_volume                  40
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C82 H69 Cl O4 P2 Pd Si2, 2(C4 H8 O), C6 H12'
_chemical_formula_sum            'C96 H99 Cl O6 P2 Pd Si2'
_chemical_formula_weight         1608.72
_chemical_name_systematic
;
?
;
_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                 114.0080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.5371(3)
_cell_length_b                   23.2484(5)
_cell_length_c                   14.3898(3)
_cell_measurement_reflns_used    147708
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.32
_cell_measurement_theta_min      2.34
_cell_volume                     4136.92(16)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker ShelXTL'
_computing_publication_material  'Bruker ShelXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex II kappa 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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            147604
_diffrn_reflns_theta_full        33.32
_diffrn_reflns_theta_max         33.32
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  0.9544
_exptl_absorpt_correction_T_min  0.8359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, G.M., 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.531
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1036
_refine_ls_number_reflns         31588
_refine_ls_number_restraints     277
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0613P)^2^+1.1792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                29279
_reflns_number_total             31588
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10356c.txt
_cod_data_source_block           10c
_cod_original_cell_volume        4136.91(15)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7016385