Chiral palladacycles based on resorcinol monophosphite ligands: the role of the meta-hydroxyl in ligand C-H activation and catalysis.
Bedford, Robin B.; Chang, Yu-Ning; Haddow, Mairi F.; McMullin, Claire L.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 9042–9050; doi:10.1039/c1dt10357a

data_7016389
_publ_section_title
;
 Chiral palladacycles based on resorcinol monophosphite ligands: the
 role of the meta-hydroxyl in ligand C-H activation and catalysis.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9042
_journal_page_last               9050
_journal_paper_doi               10.1039/c1dt10357a
_journal_volume                  40
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H48 Cl2 O4 P Pd Si2, C6 H16 N'
_chemical_formula_sum            'C46 H64 Cl2 N O4 P Pd Si2'
_chemical_formula_weight         959.43
_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                 105.2860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.1630(4)
_cell_length_b                   14.3800(2)
_cell_length_c                   14.1182(2)
_cell_measurement_reflns_used    77077
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      2.34
_cell_volume                     5319.53(13)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            77077
_diffrn_reflns_theta_full        30.60
_diffrn_reflns_theta_max         30.60
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.9460
_exptl_absorpt_correction_T_min  0.7015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, G.M., 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The discordered solvent is likely to be pentane. The electron count may not
be accurate; three low angle reflections are missing.
;
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         16225
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0397P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                14689
_reflns_number_total             16225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10357a.txt
_cod_data_source_block           yc4_26squeeze
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7016389