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_7001120
_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         'C24 H38 N4 O4 Pd2 S, 6(H2 O)'
_chemical_formula_sum            'C24 H50 N4 O10 Pd2 S'
_chemical_formula_weight         799.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 91.169(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9056(3)
_cell_length_b                   24.7652(5)
_cell_length_c                   15.04568(13)
_cell_measurement_reflns_used    22704
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.13
_cell_volume                     3317.62(13)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Mergehklf5'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0879
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36548
_diffrn_reflns_theta_full        27.71
_diffrn_reflns_theta_max         27.71
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.846
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         12407
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+12.0199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                12212
_reflns_number_total             12407
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b816936e.txt
_cod_data_source_block           s3461a
_cod_original_cell_volume        3317.61(13)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7001120