Synthesis, characterisation and catalytic investigation of a new type of PC(sp3)P pincer Pd(II) complex
Sven Sjövall; Ola F. Wendt; Carlaxel Andersson; J. Chem. Soc., Dalton Trans.  (2002) 1396–1400; doi:10.1039/b111487p

data_7011431
_publ_section_title
;
 Synthesis, characterisation and catalytic investigation of a new type
 of PC(sp3)P pincer Pd(II) complex
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1396
_journal_page_last               1400
_journal_paper_doi               10.1039/b111487p
_journal_year                    2002
_chemical_formula_sum            'C24 H49 I P2 Pd'
_chemical_formula_weight         632.87
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.27(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.102(2)
_cell_length_b                   15.035(3)
_cell_length_c                   15.875(3)
_cell_measurement_reflns_used    5959
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      49.994
_cell_measurement_theta_min      4.363
_cell_volume                     2842.2(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond (Brandenburg)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29034
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.00
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    1.860
_exptl_absorpt_correction_T_max  0.7904
_exptl_absorpt_correction_T_min  0.6624
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'absorption corrections using SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.824
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         8936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.824
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0448
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1566
_reflns_number_gt                4782
_reflns_number_total             8936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111487p.txt
_cod_data_source_block           B111487P
_cod_original_cell_volume        2842.3(10)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7011431