Sulfato-bridged ECE-pincer palladium(ii) complexes: structures in the solid-state and in solution, and catalytic properties
Kruithof, Cornelis A.; Berger, Alexsandro; Dijkstra, Harmen P.; Soulimani, Fouad; Visser, Tom; Lutz, Martin; Spek, Anthony L.; Gebbink, Robertus J. M. Klein; van Koten, Gerard; Dalton Transactions  (2009) 3306–3314; doi:10.1039/b816936e

data_7001119
_publ_section_title
;
 Sulfato-bridged ECE-pincer palladium(ii) complexes: structures in the
 solid-state and in solution, and catalytic properties
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              3306
_journal_page_last               3314
_journal_paper_doi               10.1039/b816936e
_journal_year                    2009
_chemical_formula_moiety         'C32 H50 O4 Pd2 S5, 2(H2 O)'
_chemical_formula_sum            'C32 H54 O6 Pd2 S5'
_chemical_formula_weight         907.85
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.700(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5104(6)
_cell_length_b                   14.0482(6)
_cell_length_c                   17.2217(13)
_cell_measurement_reflns_used    273
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.38
_cell_measurement_theta_min      4.36
_cell_volume                     3674.5(4)
_computing_cell_refinement       Dirax
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-97 (Beurskens et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35292
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1999)'
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         4226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0191
_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^)+(0.0224P)^2^+5.1256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0464
_reflns_number_gt                3797
_reflns_number_total             4226
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b816936e.txt
_cod_data_source_block           s3028a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7001119