Molecular Catenation via Metal-Directed Self-Assembly and π-Donor/π-Acceptor Interactions: Efficient One-Pot Synthesis, Characterization, and Crystal Structures of [3]Catenanes Based on Pd or Pt Dinuclear Metallocycles
Víctor Blanco; Marcos Chas; Dolores Abella; Carlos Peinador; José M. Quintela; Journal of the American Chemical Society 129 (2007) 13978–13986; doi:10.1021/ja074721a

data_4110154
_publ_section_title
;
 Molecular Catenation via Metal-Directed Self-Assembly and
 \p-Donor/\p-Acceptor Interactions: Efficient One-Pot Synthesis,
 Characterization, and Crystal Structures of [3]Catenanes Based on Pd or
 Pt Dinuclear Metallocycles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13978
_journal_page_last               13986
_journal_paper_doi               10.1021/ja074721a
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C112 H132 F29 N12 O42 P4 Pd2 S4'
_chemical_formula_weight         3334.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.237(4)
_cell_angle_beta                 78.635(4)
_cell_angle_gamma                79.900(4)
_cell_formula_units_Z            2
_cell_length_a                   18.292(3)
_cell_length_b                   20.433(3)
_cell_length_c                   20.878(3)
_cell_measurement_reflns_used    14122
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.622
_cell_measurement_theta_min      4.669
_cell_volume                     7362.8(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.1041
_diffrn_reflns_av_sigmaI/netI    0.1551
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            97592
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.9341
_exptl_absorpt_correction_T_min  0.8231
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             3402
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.971
_refine_diff_density_min         -1.548
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.340
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1836
_refine_ls_number_reflns         35755
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.343
_refine_ls_R_factor_all          0.2740
_refine_ls_R_factor_gt           0.1589
_refine_ls_shift/su_max          4.596
_refine_ls_shift/su_mean         0.111
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4089
_refine_ls_wR_factor_ref         0.4637
_reflns_number_gt                14672
_reflns_number_total             35755
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074721asi20070713_011116.cif
_cod_data_source_block           pvb70c
_cod_original_cell_volume        7363(2)
_cod_database_code               4110154