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_7016381
_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_formula_moiety         'C60 H50 O4 Si2'
_chemical_formula_sum            'C60 H50 O4 Si2'
_chemical_formula_weight         891.18
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9481(4)
_cell_length_b                   17.2684(6)
_cell_length_c                   31.2989(12)
_cell_measurement_reflns_used    8612
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.13
_cell_measurement_theta_min      2.36
_cell_volume                     5376.8(4)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            12378
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
Solvents used in recrystallisation were dichloromethane and diethyl ether. It
was not possible to identify the solvent from the residual electron density
map. The electron count suggested by SQUEEZE suggests an extra four
molecule of dichloromethane or diethylether per unit cell.
;
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.23(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         12378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0984P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1535
_reflns_number_gt                9896
_reflns_number_total             12378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10356c.txt
_cod_data_source_block           6dsqueeze
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7016381