A novel linkage-isomeric pair of dinuclear Pd(II) complexes bearing a bis-bidentate tetraphos ligand
Fessler, Markus; Czermak, Georg; Eller, Sylvia; Trettenbrein, Barbara; Brüggeller, Peter; Bettucci, Lorenzo; Bianchini, Claudio; Meli, Andrea; Ienco, Andrea; Oberhauser, Werner; Dalton Transactions  (2009) 1859–1869; doi:10.1039/b815392b

data_7000636
_publ_section_title
;
 A novel linkage-isomeric pair of dinuclear Pd(II) complexes bearing a
 bis-bidentate tetraphos ligand
;
_journal_coden_ASTM              DTARAF
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              1859
_journal_page_last               1869
_journal_paper_doi               10.1039/b815392b
_journal_year                    2009
_chemical_formula_moiety
'C60 H60 Cl4 O8 P4 Pd2, C2 H4 Cl2, C1.60 Cl1.60, C2 Cl2'
_chemical_formula_sum            'C65.6 H64 Cl9.6 O8 P4 Pd2'
_chemical_formula_weight         1657.37
_chemical_name_common            (Pd2Cl4(o-MeO-dppcb))
_chemical_name_systematic        '[Pd2Cl4(o-MeO-dppcb)]'
_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                 90.568(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3220(4)
_cell_length_b                   12.3410(3)
_cell_length_c                   46.756(1)
_cell_measurement_reflns_used    88241
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.998
_cell_volume                     7109.6(3)
_computing_cell_refinement       'Denzo and Scalepack'
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'Denzo and Scalepack'
_computing_molecular_graphics    'SHELXTL-NT V6.1'
_computing_publication_material  'SHELXTL-NT V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measurement_device_type  'Kappa CCD'
_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  0.0290
_diffrn_reflns_av_sigmaI/netI    0.2376
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            23218
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Otwinowski et al, 1997'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3347.2
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         12414
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0865P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.2078
_reflns_number_gt                5251
_reflns_number_total             12414
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            B815392b.txt
_cod_data_source_block           1a6
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C65.60 H64 Cl9.60 O8 P4 Pd2'
_cod_database_code               7000636
_diffrn_measured_fraction        0.995