Dinuclear palladium(II) compounds with bridging cyclometalated phosphines. Synthesis, crystal structure and electrochemical study.
Koshevoy, Igor O.; Lahuerta, Pascual; Sanaú, Mercedes; Ubeda, M. Angeles; Doménech, Antonio; Dalton transactions (Cambridge, England : 2003)  (2006) 5536–5541; doi:10.1039/b609829k

data_7007745
_publ_section_title
;
 Dinuclear palladium(II) compounds with bridging cyclometalated
 phosphines. Synthesis, crystal structure and electrochemical study.
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_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5536
_journal_page_last               5541
_journal_paper_doi               10.1039/b609829k
_journal_year                    2006
_chemical_formula_sum            'C46 H46 O4 P2 Pd2'
_chemical_formula_weight         937.57
_chemical_name_systematic
;
?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                   10.9390(3)
_cell_length_b                   15.9320(4)
_cell_length_c                   23.5800(6)
_cell_measurement_reflns_used    19592
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     4109.53(19)
_computing_cell_refinement       'HKL Scalepak (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'Denzo & Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker AXS)'
_computing_publication_material  'SHELXTL 6.10 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.3205
_diffrn_reflns_av_sigmaI/netI    0.1742
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            20460
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.882
_refine_diff_density_min         -1.817
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       0.0020(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.0958
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1720P)^2^+6.1899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2549
_refine_ls_wR_factor_ref         0.3301
_reflns_number_gt                2649
_reflns_number_total             4694
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b609829k.txt
_cod_data_source_block           Compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorombic' was replaced with
'orthorhombic' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               7007745